dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
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large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-524f8dc4a789487889bf25d15554823c
COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1cc([N+](=O)[O-])cc([N+](=O)[O-])c1)C3>>COc1ccc2[nH]c3cc(-c4cc([N+](=O)[O-])cc([N+](=O)[O-])c4)c4c(c3c2c1)C(=O)NC4=O
[N+](=O)([O-])C=1C=C(C=C(C1)[N+](=O)[O-])C1CC=2NC=3C=CC(=CC3C2C2C1C(NC2=O)=O)OC.C(#N)C1=C(C(=O)C(=C(C1=O)Cl)Cl)C#N>>[N+](=O)([O-])C=1C=C(C=C(C1)[N+](=O)[O-])C1=CC=2NC=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]3[c:25]([c:26]2[cH:27]1)[CH:24]1[CH:23]([CH:10]([c:11]2[cH:12][c:13]([N+:14](=[O:15])[O-:16])[cH:17][c:18]([N+:19](=[O:20])[O-:21])[cH:22]2)[CH2:9]3)[C:31](=[O:32])[NH:30][C:28]1=[O:29]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]3[cH:9][c:10](-[c:11]4[cH:12][c:13]([N+...
COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1cc([N+](=O)[O-])cc([N+](=O)[O-])c1)C3
COc1ccc2[nH]c3cc(-c4cc([N+](=O)[O-])cc([N+](=O)[O-])c4)c4c(c3c2c1)C(=O)NC4=O
null
null
null
Oxidation
OtherReaction
3d157ee1e52021ba4f102c0e4bf23d31153db03cc8f65d6ae2d3bbc53db1b830
82a3692de44364afcfd8cc4460435180e0752c31812bf6008d75e02664a32947
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
[O;D1;H0:1]=[C:2]1-[#7:3]-[C:4](=[O;D1;H0:5])-[CH;D3;+0:6]2-[CH;D3;+0:7](-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12])-[CH2;D2;+0:13]-[c:14]3:[#7;a:15]:[c:16]:[c:17]:[c:18]:3-[CH;D3;+0:19]-1-2>>[O;D1;H0:1]=[C:2]1-[#7:3]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:6]2:[c;H0;D3;+0:7](-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]):[cH...
42
[{"value": 42.0, "product": "[N+](=O)([O-])C=1C=C(C=C(C1)[N+](=O)[O-])C1=CC=2NC=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The reaction of 4-(3,5-Dinitrophenyl)-9-methoxy-4,5,6,10c-tetrahydropyrrolo[3,4-c]carbazole-1,3(2H,3aH)-dione (IV; Ar=3,5-dinitrophenyl, R═H) (41) prepared as described in example 47 with DDQ according to the procedure described in example 70 gave 4-(3,5-dinitrophenyl)-9-methoxypyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione ...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c3c([nH]c2c1)CCC1CNCC31
c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
null
null
null
null
COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1cc([N+](=O)[O-])cc([N+](=O)[O-])c1)C3>>COc1ccc2[nH]c3cc(-c4cc([N+](=O)[O-])cc([N+](=O)[O-])c4)c4c(c3c2c1)C(=O)NC4=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9646ed85d1e945ff98b8b534569f0755
COc1ccc2[nH]c3cc(-c4cc([N+](=O)[O-])cc([N+](=O)[O-])c4)c4c(c3c2c1)C(=O)NC4=O>>O=C1NC(=O)c2c1c(-c1cc([N+](=O)[O-])cc([N+](=O)[O-])c1)cc1[nH]c3ccc(O)cc3c21
[N+](=O)([O-])C=1C=C(C=C(C1)[N+](=O)[O-])C1=CC=2NC=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC.Cl.[NH+]1=CC=CC=C1>>[N+](=O)([O-])C=1C=C(C=C(C1)[N+](=O)[O-])C1=CC=2NC=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O
C[O:28][c:27]1[cH:26][cH:25][c:24]2[nH:23][c:22]3[cH:21][c:8](-[c:9]4[cH:10][c:11]([N+:12](=[O:13])[O-:14])[cH:15][c:16]([N+:17](=[O:18])[O-:19])[cH:20]4)[c:7]4[c:6]([c:31]3[c:30]2[cH:29]1)[C:4](=[O:5])[NH:3][C:2]4=[O:1]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][c:11]([N+:12](=[O:13])[O-:14])[cH:...
COc1ccc2[nH]c3cc(-c4cc([N+](=O)[O-])cc([N+](=O)[O-])c4)c4c(c3c2c1)C(=O)NC4=O
O=C1NC(=O)c2c1c(-c1cc([N+](=O)[O-])cc([N+](=O)[O-])c1)cc1[nH]c3ccc(O)cc3c21
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
57
[{"value": 57.0, "product": "[N+](=O)([O-])C=1C=C(C=C(C1)[N+](=O)[O-])C1=CC=2NC=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The reaction of 4-(3,5-dinitrophenyl)-9-methoxypyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (V; Ar=3,5-dinitrophenyl, R10═H) (42) prepared as described in example 48 with pyridinium hydrochloride according to the proceedure described in example 81 gave 4-(3,5-Dinitrophenyl)-9-hydroxypyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3
Other
null
null
null
COc1ccc2[nH]c3cc(-c4cc([N+](=O)[O-])cc([N+](=O)[O-])c4)c4c(c3c2c1)C(=O)NC4=O>>O=C1NC(=O)c2c1c(-c1cc([N+](=O)[O-])cc([N+](=O)[O-])c1)cc1[nH]c3ccc(O)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-26238d58532742e1a9fd9a0ceaebf033
COc1ccc2c(c1)cc(C=Cc1ccccc1OC)n2CCCO[Si](C)(C)C(C)(C)C.O=C1C=CC(=O)N1>>COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12
C1(C=CC(N1)=O)=O.[Si](C)(C)(C(C)(C)C)OCCCN1C(=CC2=CC(=CC=C12)OC)C=CC1=C(C=CC=C1)OC>>[Si](C)(C)(C(C)(C)C)OCCCN1C=2C=CC(=CC2C=2C3C(C(CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[cH:9][c:10]([CH:23]=[CH:24][c:25]1[cH:26][cH:27][cH:28][cH:29][c:30]1[O:31][CH3:32])[n:11]2[CH2:12][CH2:13][CH2:14][O:15][Si:16]([CH3:17])([CH3:18])[C:19]([CH3:20])([CH3:21])[CH3:22].[CH:33]1=[CH:39][C:37](=[O:38])[NH:36][C:34]1=[O:35]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c...
COc1ccc2c(c1)cc(C=Cc1ccccc1OC)n2CCCO[Si](C)(C)C(C)(C)C.O=C1C=CC(=O)N1
COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12
null
null
null
C-C Coupling
OtherReaction
cb72f4a0e87703d4feb5445ea9e00fcafa1b033ce261ae8123af01ad6ee77064
410ec9b1cc243569e4ff568c248f0b402403802e002b4018f576af3f6960507b
O=C1NC(=O)C2C(c3ccccc3)Cc3[nH]c4ccccc4c3C12
[C:1]-[#7;a:2]1:[c:3](-[CH;D2;+0:4]=[CH;D2;+0:5]-[c:6](:[c:7]):[c:8]):[cH;D2;+0:9]:[c:10](:[c:11]):[c:12]:1:[c:13].[O;D1;H0:14]=[C:15]1-[#7:16]-[C:17](=[O;D1;H0:18])-[CH;D2;+0:19]=[CH;D2;+0:20]-1>>[C:1]-[#7;a:2]1:[c:3]2:[c;H0;D3;+0:9](:[c:10](:[c:11]):[c:12]:1:[c:13])-[CH;D3;+0:19]1-[C:17](=[O;D1;H0:18])-[#7:16]-[C:15]...
89
[{"value": 89.0, "product": "[Si](C)(C)(C(C)(C)C)OCCCN1C=2C=CC(=CC2C=2C3C(C(CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The reaction of 1-(3-{[tert-Butyl(dimethyl)silyl]oxy}propyl)-5-methoxy-2-[2-(2-methoxyphenyl)ethenyl]-1H-indole (III; Ar=2-methoxyphenyl, R10═CH2CH2CH2OSiMe2t-Bu) (98) prepared as described in example 51 with maleimide using the procedure described in example 68 gave 6-(3-{[tert-Butyl(dimethyl)silyl]oxy}propyl)-9-metho...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2[nH]ccc2c1.C1=CCNC1
C1NCC2c3c([nH]c4ccccc34)C[CH]C12
c1ccccc1.C1NCC2c3c([nH]c4ccccc34)C[CH]C12
null
null
null
null
COc1ccc2c(c1)cc(C=Cc1ccccc1OC)n2CCCO[Si](C)(C)C(C)(C)C.O=C1C=CC(=O)N1>>COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1860bb7aaf754f549fac96415c1c1103
COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4OC)cc1n2CCCO)C(=O)NC3=O
[Si](C)(C)(C(C)(C)C)OCCCN1C=2C=CC(=CC2C=2C3C(C(CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC.C(#N)C1=C(C(=O)C(=C(C1=O)Cl)Cl)C#N.Cl>>OCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC
CC(C)(C)[Si](C)(C)[O:27][CH2:26][CH2:25][CH2:24][n:23]1[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8][c:7]2[c:9]2[c:22]1[CH2:21][CH:12]([c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[O:19][CH3:20])[CH:11]1[CH:10]2[C:31](=[O:32])[NH:30][C:28]1=[O:29]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[c:9]1[c:10]3[c:11]([c:12]...
COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12
COc1ccc2c(c1)c1c3c(c(-c4ccccc4OC)cc1n2CCCO)C(=O)NC3=O
null
null
C1CCOC1.CO
Miscellaneous
OtherReaction
6c9712e00c7b4d1c5f8a072ac030d252cf1631f2fe61823cdac905a14569b28d
8810278526f6a2c0e6c6bc11dce581d57652dfa7eee92b5b7a2e8cacd394ef1e
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2]-[C:3]-[C:4]-[#7;a:5]1:[c:6]:[c:7]:[c:8]2:[c:9]:1-[CH2;D2;+0:10]-[CH;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15](-[#8:16]):[c:17])-[CH;D3;+0:18]1-[C:19](=[O;D1;H0:20])-[#7:21]-[C:22](=[O;D1;H0:23])-[CH;D3;+0:24]-1-2>>[#8:16]-[c:15](:[c:17]):[c;H0;D3;+0:12](-[c;H0;D3;+0...
72
[{"value": 72.0, "product": "OCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The reaction of 6-(3-{[tert-Butyl(dimethyl)silyl)oxy}propyl)-9-methoxy-4-(2-methoxyphenyl)-4,5,6,10c-tetrahydropyrrolo[3,4-c]carbazole-1,3(2H,3aH)-dione (IV; Ar=2-methoxyphenyl; R10═CH2CH2CH2OSiMe2t-Bu) prepared as described in example 52 with DDQ using the procedure described in example 70 followed reaction with 2N HC...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Primary alcohol
C1NCC2c3c([nH]c4ccccc34)C[CH]C12
C1NCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
C1CCOC1.CO
null
null
COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12>C1CCOC1.CO>COc1ccc2c(c1)c1c3c(c(-c4ccccc4OC)cc1n2CCCO)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8c86a68d22c44256bfbf666ba786b6a7
COc1ccc2c(c1)c1c3c(c(-c4ccccc4OC)cc1n2CCCO)C(=O)NC3=O>>O=C1NC(=O)c2c1c(-c1ccccc1O)cc1c2c2cc(O)ccc2n1CCCO
B(Br)(Br)Br.OCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCO)C1=C(C=CC=C1)O)C(NC4=O)=O
C[O:15][c:14]1[c:9](-[c:8]2[c:7]3[c:6]([c:18]4[c:17]([cH:16]2)[n:26]([CH2:27][CH2:28][CH2:29][OH:30])[c:25]2[c:19]4[cH:20][c:21]([O:22]C)[cH:23][cH:24]2)[C:4](=[O:5])[NH:3][C:2]3=[O:1])[cH:10][cH:11][cH:12][cH:13]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[OH:15])[cH:1...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4OC)cc1n2CCCO)C(=O)NC3=O
O=C1NC(=O)c2c1c(-c1ccccc1O)cc1c2c2cc(O)ccc2n1CCCO
null
null
null
Deprotection
OtherReaction
a0f05885bbc65ae2846cad0ac34029941211b2ef3a426958b0c8aa83bb16fe86
9df751cd682ad9d54ed75d7313aaead6a019c5d37ede15c4672866d319b900ff
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].C-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]
82
[{"value": 82.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCO)C1=C(C=CC=C1)O)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The reaction of 6-(3-Hydroxypropyl)-9-methoxy-4-(2-methoxyphenyl)pyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (V; Ar=2-methoxyphenyl, R10═CH2CH2CH2OH) (100) prepared as described in example 53 with BBr3 using the procedure described in example 80 gave 9-Hydroxy-4-(2-hydroxyphenyl)-6-(3-hydroxypropyl)pyrrolo[3,4-c]carbazole...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Aromatic alcohol.Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
Other
null
null
null
COc1ccc2c(c1)c1c3c(c(-c4ccccc4OC)cc1n2CCCO)C(=O)NC3=O>>O=C1NC(=O)c2c1c(-c1ccccc1O)cc1c2c2cc(O)ccc2n1CCCO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f0c7b50e2fa14884897237926ba5e44f
COc1ccc2c(c1)cc(C=Cc1c(Cl)cccc1OC)n2CCCO[Si](C)(C)C(C)(C)C.O=C1C=CC(=O)N1>>COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1c(Cl)cccc1OC)C3.COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12
[Si](C)(C)(C(C)(C)C)OCCCN1C(=CC2=CC(=CC=C12)OC)C=CC1=C(C=CC=C1OC)Cl.C1(C=CC(N1)=O)=O>>ClC1=C(C(=CC=C1)OC)C1CC=2NC=3C=CC(=CC3C2C2C1C(NC2=O)=O)OC.[Si](C)(C)(C(C)(C)C)OCCCN1C=2C=CC(=CC2C=2C3C(C(CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[n:7]([CH2:41][CH2:42][CH2:43][O:44][Si:45]([CH3:30])([CH3:46])[C:48]([CH3:32])([CH3:54])[CH3:61])[c:8]([CH:29]=[CH:19][c:20]3[c:21]([Cl:22])[cH:23][cH:24][cH:25][c:26]3[O:27][CH3:28])[cH:9][c:10]2[cH:11]1.[CH:12]1=[CH:18][C:16](=[O:17])[NH:65][C:13]1=[O:14]>>[CH3:1][O:2][c:3]1[cH:4]...
COc1ccc2c(c1)cc(C=Cc1c(Cl)cccc1OC)n2CCCO[Si](C)(C)C(C)(C)C.O=C1C=CC(=O)N1
COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1c(Cl)cccc1OC)C3.COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12
null
null
null
Aromatic Heterocycle Formation
OtherReaction
77637d3f56cf458fa41066d1ab85ec4037cd542b079618bf456dc29c2759bfbf
e1caee8150cf72ecc4e201ba67ee2f6069c0684cf1dd043ad87dc208401efdcf
O=C1NC(=O)C2C(c3ccccc3)Cc3[nH]c4ccccc4c3C12.O=C1NC(=O)C2C(c3ccccc3)Cc3[nH]c4ccccc4c3C12
[C;D1;H3:1]-[Si;H0;D4;+0:2](-[CH3;D1;+0:3])(-[#8:4]-[C:5]-[C:6]-[CH2;D2;+0:7]-[n;H0;D3;+0:8]1:[c:9](:[c:10]):[c:11](:[c:12]):[cH;D2;+0:13]:[c:14]:1-[CH;D2;+0:15]=[CH;D2;+0:16]-[c:17](:[c:18]):[c:19])-[C;H0;D4;+0:20](-[CH3;D1;+0:21])(-[CH3;D1;+0:22])-[CH3;D1;+0:23].[O;D1;H0:24]=[C;H0;D3;+0:25]1-[CH;D2;+0:26]=[CH;D2;+0:2...
null
[]
null
null
null
null
The reaction of 1-(3-{[tert-Butyl(dimethyl)silyl]oxy}propyl)-2-[2-(2-chloro-6-methoxyphenyl)ethenyl]-5-methoxy-1H-indole (III; Ar=2-chloro-6-methoxyphenyl, R10═CH2CH2CH2OSiMe2t-Bu) (103) prepared as described in example 56 with maleimide using the procedure described in example 68 gave 6-(3-[tert-Butyl(dimethyl)silyl]o...
10.6084/m9.figshare.5104873.v1
null
Unsubstituted dicarboximide.TMS ether protective group
Ether.Ether.Unsubstituted dicarboximide.Unsubstituted dicarboximide.TMS ether protective group
c1ccc2[nH]ccc2c1.C1=CCNC1
c1ccc2c3c([nH]c2c1)CCC1CNCC31.c1ccccc1.C1NCC2c3c([nH]c4ccccc34)C[CH]C12
c1ccccc1.c1ccc2c3c([nH]c2c1)CCC1CNCC31.c1ccccc1.C1NCC2c3c([nH]c4ccccc34)C[CH]C12
Other
null
null
null
COc1ccc2c(c1)cc(C=Cc1c(Cl)cccc1OC)n2CCCO[Si](C)(C)C(C)(C)C.O=C1C=CC(=O)N1>>COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1c(Cl)cccc1OC)C3.COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2ccccc2OC)C2C(=O)NC(=O)C12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8af552d326f44e5488dc65134040e607
COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2c(Cl)cccc2OC)C2C(=O)NC(=O)C12>>COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCCO)C(=O)NC3=O
C(#N)C1=C(C(=O)C(=C(C1=O)Cl)Cl)C#N.Cl.[Si](C)(C)(C(C)(C)C)OCCCN1C=2C=CC(=CC2C=2C3C(C(CC12)C1=C(C=CC=C1OC)Cl)C(NC3=O)=O)OC.[Si](C)(C)(C(C)(C)C)OCCCN1C=2C=CC(=CC2C=2C3C(C(CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC>>ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCCO
CC(C)(C)[Si](C)(C)[O:28][CH2:27][CH2:26][CH2:25][n:24]1[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8][c:7]2[c:9]2[c:23]1[CH2:22][CH:12]([c:13]1[c:14]([Cl:15])[cH:16][cH:17][cH:18][c:19]1[O:20][CH3:21])[CH:11]1[CH:10]2[C:32](=[O:33])[NH:31][C:29]1=[O:30]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[c:9]1[c:10]3[c:11...
COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2c(Cl)cccc2OC)C2C(=O)NC(=O)C12
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCCO)C(=O)NC3=O
null
null
C1CCOC1.CO
Miscellaneous
OtherReaction
6c9712e00c7b4d1c5f8a072ac030d252cf1631f2fe61823cdac905a14569b28d
8810278526f6a2c0e6c6bc11dce581d57652dfa7eee92b5b7a2e8cacd394ef1e
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2]-[C:3]-[C:4]-[#7;a:5]1:[c:6]:[c:7]:[c:8]2:[c:9]:1-[CH2;D2;+0:10]-[CH;D3;+0:11](-[c;H0;D3;+0:12](:[c:13](-[Cl;D1;H0:14]):[c:15]):[c:16](-[#8:17]):[c:18])-[CH;D3;+0:19]1-[C:20](=[O;D1;H0:21])-[#7:22]-[C:23](=[O;D1;H0:24])-[CH;D3;+0:25]-1-2>>[#8:17]-[c:16](:[c:18]):[c;H0;D3;+0:...
76
[{"value": 76.0, "product": "ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCCO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The reaction of 6-(3-{[tert-Butyl(dimethyl)silyl]oxy}propyl)-4-(2-chloro-6-methoxyphenyl)-9-methoxy-4,5,6,10c-tetrahydropyrrolo[3,4-c]carbazole-1,3(2H,3aH)-dione (IV; Ar=2-chloro-6-methoxyphenyl, R10═CH2CH2CH2OSiMe2t-Bu) (104) prepared as described in example 57 with DDQ using the procedure described in example 70 foll...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Primary alcohol
C1NCC2c3c([nH]c4ccccc34)C[CH]C12
C1NCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
C1CCOC1.CO
null
null
COc1ccc2c(c1)c1c(n2CCCO[Si](C)(C)C(C)(C)C)CC(c2c(Cl)cccc2OC)C2C(=O)NC(=O)C12>C1CCOC1.CO>COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCCO)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-60079b1f24ca45af8dc55a802fe52b64
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCCO)C(=O)NC3=O>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO
B(Br)(Br)Br.ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCCO>>ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCO
C[O:24][c:23]1[cH:22][c:21]2[c:13]3[c:12]([cH:11][c:10](-[c:9]4[c:3]([O:2][CH3:1])[cH:4][cH:5][cH:6][c:7]4[Cl:8])[c:15]4[c:14]3[C:19](=[O:20])[NH:18][C:16]4=[O:17])[n:28]([CH2:29][CH2:30][CH2:31][OH:32])[c:27]2[cH:26][cH:25]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([Cl:8])[c:9]1-[c:10]1[cH:11][c:12]2[c:13]([c:14]3[c...
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCCO)C(=O)NC3=O
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
64
[{"value": 64.0, "product": "ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The reaction of 4-(2-Chloro-6-methoxyphenyl)-6-(3-hydroxypropyl)-9-methoxypyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (V; Ar=2-chloro-6-methoxyphenyl, R10═CH2CH2CH2OH) (105) prepared as described in example 58 with BBr3 using the procedure described in example 80 and with a reaction time of 90 minutes gave 4-(2-Chloro-6-m...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
Other
null
null
null
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCCO)C(=O)NC3=O>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fc288b67d39b4f6c88905d219fdffbcc
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO>>COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO
C(C)(=O)[O-].[K+].C(C)(=O)OCC.ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCO>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCO)C1=C(C=CC=C1)OC)C(NC4=O)=O
Cl[c:7]1[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[c:8]1-[c:9]1[cH:10][c:11]2[c:12]([c:13]3[c:14]1[C:15](=[O:16])[NH:17][C:18]3=[O:19])[c:20]1[cH:21][c:22]([OH:23])[cH:24][cH:25][c:26]1[n:27]2[CH2:28][CH2:29][CH2:30][OH:31]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1-[c:9]1[cH:10][c:11]2[c:12]([c:13]3[c:14]1[C:15](=[O...
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO
COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO
null
[Pd]
CO
Functional Group Interconversion
Aromatic dehalogenation
b66818d3926a4463fb8e1c3d4a89e94e47b4d46960d4bdb7bcfbeeec427cfd4e
56de34d4a44cb25d9380269ee5e138b0f24b40a3a0db22c5508049dc775a861f
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[c:5]):[c:6]>>[c:6]:[c:4](-[c:5]):[cH;D2;+0:1]:[c:2]:[c:3]
51
[{"value": 51.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCO)C1=C(C=CC=C1)OC)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
4-(2-Chloro-6-methoxyphenyl)-9-hydroxy-6-(3-hydroxypropyl)pyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (VI; Ar=2-chloro-6-methoxyphenyl, R10═CH2CH2CH2OH) (106) (0.20 g, 0.44 mmol) prepared as described in example 59, potassium acetate (0.20 g) and 5% Pd/C in a solution of ethyl acetate (25 ml) and methanol 1:1 (25 mL) unde...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccccc1
c1ccccc1
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
Other
[Pd].CO
null
null
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO>[Pd].CO>COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-63c40e69daaa436491abcccf68ef7925
BrCCOC1CCCCO1.CO.COc1ccc2[nH]c(C=Cc3cc([N+](=O)[O-])cc([N+](=O)[O-])c3)cc2c1.Cl>>COc1ccc2c(c1)cc(C=Cc1c(Cl)cccc1OC)n2CCO
Cl.CO.COC=1C=C2C=C(NC2=CC1)C=CC1=CC(=CC(=C1)[N+](=O)[O-])[N+](=O)[O-].O1C(CCCC1)OCCBr>>ClC1=C(C(=CC=C1)OC)C=CC=1N(C2=CC=C(C=C2C1)OC)CCO
Br[CH2:23][CH2:24][O:25]C1CCCCO1.[OH:20][CH3:21].O=[N+]([O-])[c:16]1[cH:14][c:13]([CH:12]=[CH:11][c:10]2[cH:9][c:7]3[c:6]([cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8]3)[nH:22]2)[cH:19][c:18]([N+](=O)[O-])[cH:17]1.[ClH:15]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[cH:9][c:10]([CH:11]=[CH:12][c:13]1[c:14]([Cl:15])[cH:...
BrCCOC1CCCCO1.CO.COc1ccc2[nH]c(C=Cc3cc([N+](=O)[O-])cc([N+](=O)[O-])c3)cc2c1.Cl
COc1ccc2c(c1)cc(C=Cc1c(Cl)cccc1OC)n2CCO
null
null
null
Functional Group Interconversion
OtherReaction
a419d81db6f99e9d0494792c4f406383d69616ad2500e2368e8bf456988baae9
26ce142e37b6cc0d2165819e413d601e69939fd62f0db7d84e117e5a685c3a1b
C(=Cc1cc2ccccc2[nH]1)c1ccccc1
Br-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-C1-C-C-C-C-O-1.O=[N+](-[O-])-[c;H0;D3;+0:4]1:[c:5]:[c;H0;D3;+0:6](-[N+](=O)-[O-]):[cH;D2;+0:7]:[c:8](-[C:9]=[C:10]-[c:11]2:[c:12]:[c:13]:[c:14](:[c:15]):[nH;D2;+0:16]:2):[cH;D2;+0:17]:1.[C;D1;H3:18]-[OH;D1;+0:19].[ClH;D0;+0:20]>>[C;D1;H3:18]-[O;H0;D2;+0:19]-[c;H0;D3;+0:7]1:[cH;D2;+...
91
[{"value": 91.0, "product": "ClC1=C(C(=CC=C1)OC)C=CC=1N(C2=CC=C(C=C2C1)OC)CCO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The reaction of 2-[2-(2-Chloro-6-methoxyphenyl)ethenyl]-5-methoxy-1H-indole (II; Ar=2-chloro-6-methoxyphenyl) (102) prepared as described in example 55 with 2-bromoethyl tetrahydro-2H-pyran-2-yl ether using the procedure described in example 38 followed by reaction of the crude product with 2N HCl in methanol gave 2-{2...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Nitro group.Nitro group.Methanol
Aromatic halide.Ether.Primary alcohol
C1CCOCC1.c1ccccc1.c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
c1ccc2[nH]ccc2c1.c1ccccc1
HBr
null
null
null
BrCCOC1CCCCO1.CO.COc1ccc2[nH]c(C=Cc3cc([N+](=O)[O-])cc([N+](=O)[O-])c3)cc2c1.Cl>>COc1ccc2c(c1)cc(C=Cc1c(Cl)cccc1OC)n2CCO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b19c236e376842cc819929ad988edb6a
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCO)C(=O)NC3=O>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO
B(Br)(Br)Br.ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCO>>ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCO
C[O:24][c:23]1[cH:22][c:21]2[c:13]3[c:12]([cH:11][c:10](-[c:9]4[c:3]([O:2][CH3:1])[cH:4][cH:5][cH:6][c:7]4[Cl:8])[c:15]4[c:14]3[C:19](=[O:20])[NH:18][C:16]4=[O:17])[n:28]([CH2:29][CH2:30][OH:31])[c:27]2[cH:26][cH:25]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([Cl:8])[c:9]1-[c:10]1[cH:11][c:12]2[c:13]([c:14]3[c:15]1[C:...
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCO)C(=O)NC3=O
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
56
[{"value": 56.0, "product": "ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
The reaction of 4-(2-Chloro-6-methoxyphenyl)-6-(2-hydroxyethyl)-9-methoxypyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (V; Ar=2-chloro-6-methoxyphenyl, R10═CH2CH2OH) (111) prepared as described in example 63 with BBr3 using the procedure described in example 80 except that the reaction conditions were 2 h at 0° C. gave 4-(2...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
Other
null
null
2
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCO)C(=O)NC3=O>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4f79f664c86445d28a8aee5c0bd56414
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO>>COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO
[H][H].ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCO>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCO)C1=C(C=CC=C1)OC)C(NC4=O)=O
Cl[c:7]1[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[c:8]1-[c:9]1[cH:10][c:11]2[c:12]([c:13]3[c:14]1[C:15](=[O:16])[NH:17][C:18]3=[O:19])[c:20]1[cH:21][c:22]([OH:23])[cH:24][cH:25][c:26]1[n:27]2[CH2:28][CH2:29][OH:30]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1-[c:9]1[cH:10][c:11]2[c:12]([c:13]3[c:14]1[C:15](=[O:16])[NH...
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO
COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO
null
[Pd]
null
Functional Group Interconversion
Aromatic dehalogenation
b66818d3926a4463fb8e1c3d4a89e94e47b4d46960d4bdb7bcfbeeec427cfd4e
56de34d4a44cb25d9380269ee5e138b0f24b40a3a0db22c5508049dc775a861f
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[c:5]):[c:6]>>[c:6]:[c:4](-[c:5]):[cH;D2;+0:1]:[c:2]:[c:3]
77
[{"value": 77.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCO)C1=C(C=CC=C1)OC)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of 4-(2-Chloro-6-methoxyphenyl)-9-hydroxy-6-(2-hydroxyethyl)pyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (VI; Ar-2-chloro-6-methoxyphenyl, R10═CH2CH,OH) (112) prepared as described in example 64 with hydrogen gas, using a Pd/C catalyst, according to the procedure for example 60 gave 9-Hydroxy-6-(2-hydroxyethyl)-4-...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccccc1
c1ccccc1
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
Other
[Pd]
null
null
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO>[Pd]>COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0c617c646dab4d34a16f55b00127ee4c
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCO)C(=O)NC3=O.CS(=O)(=O)Cl>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCOS(C)(=O)=O
B(Br)(Br)Br.ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCO.COC1=CC=2C=3C4=C(C(=CC3NC2C=C1)C(=O)OCC1=CC=CC=C1)C(NC4=O)=O.CS(=O)(=O)Cl>>CS(=O)(=O)OCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1OC)Cl)C(NC3=O)=O)O
C[O:24][c:23]1[cH:22][c:21]2[c:13]3[c:12]([cH:11][c:10](-[c:9]4[c:3]([O:2][CH3:1])[cH:4][cH:5][cH:6][c:7]4[Cl:8])[c:15]4[c:14]3[C:19](=[O:20])[NH:18][C:16]4=[O:17])[n:28]([CH2:29][CH2:30][OH:31])[c:27]2[cH:26][cH:25]1.Cl[S:32]([CH3:33])(=[O:34])=[O:35]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([Cl:8])[c:9]1-[c:10]1[cH...
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCO)C(=O)NC3=O.CS(=O)(=O)Cl
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCOS(C)(=O)=O
null
null
null
Acylation
OtherReaction
67bdcf4d596d39c5c19b0d52e73816be61dfa15d3d0e73b49ae2817f6b54da59
612c49341ea364c8025430031377b6efe91bae2e03711ce0a04ad7326cb56818
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]-[OH;D1;+0:7].Cl-[S;H0;D4;+0:8](-[C;D1;H3:9])(=[O;D1;H0:10])=[O;D1;H0:11]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[S;H0;D4;+0:8](-[C;D1;H3:9])(=[O;D1;H0:10])=[O;D1;H0:11].[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
Reaction of 4-(2-Chloro-6-methoxyphenyl)-6-(2-hydroxyethyl)-9-methoxypyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (V; Ar=2-chloro-6-methoxyphenyl, R10═CH2CH2OH) (111) prepared as described in example 63 with methanesulphonyl chloride, followed by reaction with BBr3 using the procedure described in example 170 of Scheme 3 g...
10.6084/m9.figshare.5104873.v1
null
Ether.Primary alcohol.Sulfonyl halide
Mesylate.Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
HCl
null
null
null
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCO)C(=O)NC3=O.CS(=O)(=O)Cl>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCOS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-915b6fcb2b644f1a8f05948a5bd18cc0
C1COCCN1.COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCOS(C)(=O)=O>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCN1CCOCC1
CS(=O)(=O)OCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1OC)Cl)C(NC3=O)=O)O.N1CCOCC1.COC1=CC=2C=3C4=C(C(=CC3NC2C=C1)C(=O)OCC1=CC=CC=C1)C(NC4=O)=O>>ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCN2CCOCC2
[NH:31]1[CH2:32][CH2:33][O:34][CH2:35][CH2:36]1.CS(=O)(=O)O[CH2:30][CH2:29][n:28]1[c:12]2[cH:11][c:10](-[c:9]3[c:3]([O:2][CH3:1])[cH:4][cH:5][cH:6][c:7]3[Cl:8])[c:15]3[c:14]([c:13]2[c:21]2[cH:22][c:23]([OH:24])[cH:25][cH:26][c:27]21)[C:19](=[O:20])[NH:18][C:16]3=[O:17]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([Cl:8])...
C1COCCN1.COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCOS(C)(=O)=O
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCN1CCOCC1
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
d65566d5f2049ef4dc70d5c480ea5af77518b25af8327af37e9d6d45c6baf558
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCN1CCOCC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[#7;a:3].[#8:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-1>>[#7;a:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[#8:4]-[C:9]-[C:8]-1
81
[{"value": 81.0, "product": "ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCN2CCOCC2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of 2-(4-(2-Chloro-6-methoxyphenyl)-9-hydroxy-1,3-dioxo-2,3-dihydropyrrolo[3,4-c]carbazol-6 (1H)-yl)ethyl methanesulfonate (VII; Ar=2-chloro-6-methoxyphenyl, n=2, mesylate) (114) prepared as described in example 66 with morpholine using the procedure described in example 179 of Scheme 3 gave 4-(2-Chloro-6-metho...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
C1COCCN1
C1COCC[NH]1
c1ccccc1.C1COCC[NH]1.C1NCc2c1ccc1nc3ccccc3c21
MsOH.HO-
null
null
null
C1COCCN1.COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCOS(C)(=O)=O>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCN1CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-94ffd459294f4be38a5e0da8180f5b07
C1CCOC1.COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O>>COc1ccc(N)cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O.COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O
C1CCOC1.Cl.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)C1=C(C=CC(=C1)[N+](=O)[O-])OC)C(NC4=O)=O.Cl>>NC=1C=CC(=C(C1)C1=CC=2NC=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)OC.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)C1=C(C=CC(=C1)[N+](=O)[O-])OC)C(NC4=O)=O
[CH2:1]1[O:2][CH2:17][CH2:34][CH2:38]1.[c:6]1([N+:7]([O-:37])=[O:55])[cH:8][c:9](-[c:10]2[cH:11][c:12]3[nH:13][c:44]4[cH:45][cH:46][c:47]([OH:48])[cH:49][c:50]4[c:21]3[c:22]3[c:23]2[C:24](=[O:25])[NH:26][C:27]3=[O:28])[c:31]([O:30][CH3:29])[cH:32][cH:33]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([NH2:7])[cH:8][c:9]1-[c:10]...
C1CCOC1.COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O
COc1ccc(N)cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O.COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O
null
B#[Ni]
CO
Aromatic Heterocycle Formation
OtherReaction
24cb48caead4af5477eb428d6a329c00acbc966b236385afa426c1e363a355a6
e8ec873f1d7d2668181feaf329978a3d2ba96201f1f0a58688fd21dc7ebce832
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21.O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
[C;D1;H3:1]-[#8:2]-[c;H0;D3;+0:3]1:[c:4]:[cH;D2;+0:5]:[c;H0;D3;+0:6](-[N+;H0;D3:7](-[O-;H0;D1:8])=[O;H0;D1;+0:9]):[c:10]:[c;H0;D3;+0:11]:1-[c:12]1:[c:13]:[c:14]2:[nH;D2;+0:15]:[c;H0;D3;+0:16]3:[c:17]:[c:18]:[c:19]:[c:20]:[c;H0;D3;+0:21]:3:[c;H0;D3;+0:22]:2:[c:23]2:[c:24]:1-[C:25](=[O;D1;H0:26])-[#7:27]-[C:28]-2=[O;D1;H...
null
[]
60
CELSIUS
null
null
To a solution of 9-hydroxy-4-(2-methoxy-5-nitrophenyl)pyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (VI; Ar=2-methoxy-5-nitrophenyl, R10═H) (38) (64 mg, 0.159 mmol) prepared according to example 72 in methanol (10 mL) and THF (1 mL) was added 2N HCl (1 mL) Freshly prepared nickel boride (˜0.50 g) was added and the mixture w...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Nitro group
Ether.Ether.Unsubstituted dicarboximide.Nitro group.Aromatic alcohol.Primary amine
C1CCOC1.c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3.c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3.c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
Other
B#[Ni].CO
60
null
C1CCOC1.COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O>B#[Ni].CO>COc1ccc(N)cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O.COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-624945cdd7dc40bf82e1a9c34cf99862
COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1ccccc1Cl)C3>>COc1ccc2[nH]c3cc(-c4ccccc4Cl)c4c(c3c2c1)C(=O)NC4=O
ClC1=C(C=CC=C1)C1CC=2NC=3C=CC(=CC3C2C2C1C(NC2=O)=O)OC.[Si](C)(C)(C(C)(C)C)OCCCN1C=2C=CC(=CC2C=2C3C(C(CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)OC.ClC1=C(C=CC=C1)C1CC=2NC=3C=CC(=CC3C2C2C1C(NC2=O)=O)OC>>ClC1=C(C=CC=C1)C1=CC=2NC=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]3[c:20]([c:21]2[cH:22]1)[CH:19]1[CH:18]([CH:10]([c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[Cl:17])[CH2:9]3)[C:26](=[O:27])[NH:25][C:23]1=[O:24]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]3[cH:9][c:10](-[c:11]4[cH:12][cH:13][cH:14][cH:15][c:16]4[Cl:17])[c:18]4[c:19]([c...
COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1ccccc1Cl)C3
COc1ccc2[nH]c3cc(-c4ccccc4Cl)c4c(c3c2c1)C(=O)NC4=O
null
[O-2].[O-2].[Mn+4]
O1CCOCC1
Oxidation
OtherReaction
3d157ee1e52021ba4f102c0e4bf23d31153db03cc8f65d6ae2d3bbc53db1b830
82a3692de44364afcfd8cc4460435180e0752c31812bf6008d75e02664a32947
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[CH;D3;+0:5]1-[CH2;D2;+0:6]-[c:7]2:[#7;a:8]:[c:9]:[c:10]:[c:11]:2-[CH;D3;+0:12]2-[C:13](=[O;D1;H0:14])-[#7:15]-[C:16](=[O;D1;H0:17])-[CH;D3;+0:18]-1-2):[c:19]:[c:20]>>[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[c;H0;D3;+0:5]1:[cH;D2;+0:6]:[c:7]2:[#7;a:8]:[c:9]:[c:10]:[c:11]:2:...
null
[]
null
null
16
HOUR
Manganese dioxide (12.0 g) was added to a solution of 4-(2-Chlorophenyl)-9-methoxy-4,5,6,10c-tetrahydropyrrolo[3,4-c]carbazole-1,3(2H,3aH)-dione (IV; Ar=2-chlorophenyl, R10═H (32) prepared as described in example 68 (2.1 g, 5.51 mmol) in dioxane (100 mL) and the mixture was refluxed with stirring for 16 h. The mixture ...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c3c([nH]c2c1)CCC1CNCC31
c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
null
[O-2].[O-2].[Mn+4].O1CCOCC1
null
16
COc1ccc2[nH]c3c(c2c1)C1C(=O)NC(=O)C1C(c1ccccc1Cl)C3>[O-2].[O-2].[Mn+4].O1CCOCC1>COc1ccc2[nH]c3cc(-c4ccccc4Cl)c4c(c3c2c1)C(=O)NC4=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8ee1968d724d49868e7cadce4af9eada
COc1ccc2[nH]c(C=Cc3cc([N+](=O)[O-])cc([N+](=O)[O-])c3)cc2c1.COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCCO)C(=O)NC3=O.O=C([O-])O>>COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O.O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCO
B(Br)(Br)Br.ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCCO.C(=O)(O)[O-].[Na+].O.COC=1C=C2C=C(NC2=CC1)C=CC1=CC(=CC(=C1)[N+](=O)[O-])[N+](=O)[O-]>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCO.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)C1=C(C=CC(=C1)[N+](=O)[O-])OC)C(NC4=O)=O
[O-][N+:33]([c:4]1[cH:5][c:6]([N+:7](=[O:8])[O-:9])[cH:10][c:11]([CH:12]=[CH:13][c:14]2[nH:15][c:16]3[cH:17][cH:18][c:19]([O:2][CH3:1])[cH:21][c:22]3[cH:23]2)[cH:24]1)=[O:35].[CH3:3][O:52][c:51]1[cH:50][c:49]2[c:48]3[c:36]4[c:37]([c:38](-[c:39]5[cH:40][cH:41][cH:42][cH:43][c:44]5[Cl:45])[cH:46][c:47]3[n:56]([CH2:57][CH...
COc1ccc2[nH]c(C=Cc3cc([N+](=O)[O-])cc([N+](=O)[O-])c3)cc2c1.COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCCO)C(=O)NC3=O.O=C([O-])O
COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O.O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCO
null
null
C(Cl)Cl
Aromatic Heterocycle Formation
OtherReaction
b0aa36dc88b7b8fc7b234668e1ea4dbf66580ec1eca181530addacc47e8e098f
285b97627062e5437bdecc02dda67f0b12cb80b7e2a471ada0633a465c5f92dc
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21.O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
O-[C;H0;D3;+0:1](-[O-;H0;D1:2])=[O;D1;H0:3].[C;D1;H3:4]-[O;H0;D2;+0:5]-[c;H0;D3;+0:6]1:[c:7]:[c:8]:[c:9]2:[#7;a:10]:[c:11](-[CH;D2;+0:12]=[CH;D2;+0:13]-[c;H0;D3;+0:14]3:[c:15]:[c:16]:[c:17]:[c;H0;D3;+0:18](-[N+;H0;D3:19](-[O-])=[O;H0;D1;+0:20]):[cH;D2;+0:21]:3):[cH;D2;+0:22]:[c:23]:2:[c:24]:1.[C:25]-[#7;a:26]1:[c:27]:[...
null
[]
null
null
3
HOUR
A solution of 1N BBr3 in CH2Cl2 (11.5 mL, 0.011 mol) was added to a solution of 4-(2-Chlorophenyl)-6-(3-hydroxypropyl)-9-methoxypyrrolo[3,4-c]carbazole-1,3(2H,6H)-dione (V; Ar=2-chlorophenyl, R10═CH2CH2CH2OH) (31) prepared as described in example 40 (1.00 g, 2.30 mmol) in CH2Cl2 under nitrogen and the reaction mixture ...
10.6084/m9.figshare.5104873.v1
null
Carbonic Acid.Ether.Ether.Unsubstituted dicarboximide.Nitro group
Ether.Unsubstituted dicarboximide.Unsubstituted dicarboximide.Aromatic alcohol.Aromatic alcohol
c1ccccc1.c1ccc2[nH]ccc2c1.C1NCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3.C1NCc2c1ccc1nc3ccccc3c21
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3.c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
null
C(Cl)Cl
null
3
COc1ccc2[nH]c(C=Cc3cc([N+](=O)[O-])cc([N+](=O)[O-])c3)cc2c1.COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCCO)C(=O)NC3=O.O=C([O-])O>C(Cl)Cl>COc1ccc([N+](=O)[O-])cc1-c1cc2[nH]c3ccc(O)cc3c2c2c1C(=O)NC2=O.O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3f6e1d2b349c474fa6a16a0f93f62613
BrCCOC1CCCCO1.COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Br)cc2c1.O=C1C=CC(=O)N1>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCO)C(=O)NC3=O
C1(=CC=C(C=C1)S(=O)(=O)O)C.BrC1=C(C=CC(=C1)[N+](=O)[O-])/C=C/C=1NC2=CC=C(C=C2C1)OC.BrCCOC1OCCCC1.C1(C=CC(N1)=O)=O>>OCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)OC
Br[CH2:22][CH2:23][O:24][CH:13]1O[CH2:17][CH2:16][CH2:15][CH2:14]1.O=[N+]([O-])c1c[cH:10][c:11](/[CH:12]=[CH:19]/[c:20]2[cH:9][c:7]3[c:6]([cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8]3)[nH:21]2)[c:18](Br)c1.C1=C[C:28](=[O:29])[NH:27][C:25]1=[O:26]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[c:9]1[c:10]3[c:11]([c:12](-[...
BrCCOC1CCCCO1.COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Br)cc2c1.O=C1C=CC(=O)N1
COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCO)C(=O)NC3=O
null
null
CO.O
Functional Group Interconversion
OtherReaction
6e82cd7df1922012ed4baa109595c52e05a2e1d183aad57859993f24b4d960a7
429670d348dbe5d5eb00efb5ffc8485353034416000e99d901dbdc174ea1ab0e
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Br-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-[CH;D3;+0:4]1-O-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[CH2;D2;+0:7]-[CH2;D2;+0:8]-1.Br-[c;H0;D3;+0:9]1:c:c(-[N+](=O)-[O-]):c:[cH;D2;+0:10]:[c;H0;D3;+0:11]:1/[CH;D2;+0:12]=[CH;D2;+0:13]/[c:14]1:[cH;D2;+0:15]:[c:16](:[c:17]):[c:18](:[c:19]):[nH;D2;+0:20]:1.[O;D1;H0:21]=[C;H0;D3;+0:22]1-C=C-[C;...
null
[]
50
CELSIUS
null
null
5-methoxy-2-[(E,Z)-2-phenylethenyl]-1H-indole (II; Ar=phenyl) (1.93 g, 7.74 mmol was reacted with 2-(2-bromoethoxy)tetrahydro-2H-pyran using the procedure described in example 38. This material was reacted directly with maleimide (0.79 g) using the procedure described in method 4. The product obtained was reacted using...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary halide.Ether.Ether.Unsubstituted dicarboximide.Nitro group
Unsubstituted dicarboximide.Primary alcohol
C1CCOCC1.c1ccccc1.c1ccc2[nH]ccc2c1.C1=CCNC1
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
HBr
CO.O
50
null
BrCCOC1CCCCO1.COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Br)cc2c1.O=C1C=CC(=O)N1>CO.O>COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCO)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f61fe06652e1483ba61e938ea5e32000
CC(C)(C)[Si](C)(C)OCCCBr.COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Br)cc2c1.O=C1C=CC(=O)N1>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCCO)C(=O)NC3=O
BrC1=C(C=CC(=C1)[N+](=O)[O-])/C=C/C=1NC2=CC=C(C=C2C1)OC.[Si](C)(C)(C(C)(C)C)OCCCBr.C1(C=CC(N1)=O)=O>>OCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)OC
CC(C)(C)[Si](C)(C)[O:25][CH2:24][CH2:23][CH2:22]Br.O=[N+]([O-])[c:16]1[cH:15][cH:14][c:13](/[CH:12]=[CH:19]/[c:20]2[cH:9][c:7]3[c:6]([cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8]3)[nH:21]2)[c:18](Br)[cH:17]1.[CH:10]1=[CH:11][C:26](=[O:27])[NH:28][C:29]1=[O:30]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[c:9]1[c:10]3[c:...
CC(C)(C)[Si](C)(C)OCCCBr.COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Br)cc2c1.O=C1C=CC(=O)N1
COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCCO)C(=O)NC3=O
null
null
CO.O.Cl
Aromatic Heterocycle Formation
OtherReaction
2dd49c3b4854e5e07c031b33231cdc62cc4772db06568e15427e294f7691e7a7
8f1489f5ec6e4cca230a581e53e2eec6e42dcfc20031f5625286154fafde4539
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Br-[CH2;D2;+0:1]-[C:2]-[C:3]-[O;H0;D2;+0:4]-[Si](-C)(-C)-C(-C)(-C)-C.Br-[c;H0;D3;+0:5]1:[c:6]:[c;H0;D3;+0:7](-[N+](=O)-[O-]):[c:8]:[c:9]:[c;H0;D3;+0:10]:1/[CH;D2;+0:11]=[CH;D2;+0:12]/[c:13]1:[cH;D2;+0:14]:[c:15](:[c:16]):[c:17](:[c:18]):[nH;D2;+0:19]:1.[O;D1;H0:20]=[C:21]1-[#7:22]-[C:23](=[O;D1;H0:24])-[CH;D2;+0:25]=[C...
23
[{"value": 23.0, "product": "OCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
5-Methoxy-2-[(E,Z)-2-phenylethenyl]-1H-indole (II; Ar=phenyl) (6.85 g, 27.5 mmol) was reacted with with 3-bromopropyl tert-butyl(dimethyl)silyl ether using the procedure described in example 38. The product isolated was reacted directly with maleimide (5.2 g) using the procedure described in example 68. Aromatisation o...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary halide.Nitro group.TMS ether protective group
Primary alcohol
c1ccccc1.c1ccc2[nH]ccc2c1.C1=CCNC1
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
HBr
CO.O.Cl
null
null
CC(C)(C)[Si](C)(C)OCCCBr.COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Br)cc2c1.O=C1C=CC(=O)N1>CO.O.Cl>COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCCO)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-612d771bad9043279bcecec1cba7a604
C=CC#N.COc1ccc2[nH]c(C=Cc3ccccc3Cl)cc2c1>>COc1ccc2c(c1)cc(/C=C/c1ccccc1Cl)n2CCC#N
C(C=C)#N.ClC1=C(C=CC=C1)C=CC=1NC2=CC=C(C=C2C1)OC.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)C1=C(C=CC(=C1)[N+](=O)[O-])O)C(NC4=O)=O>>ClC1=C(C=CC=C1)/C=C/C=1N(C2=CC=C(C=C2C1)OC)CCC#N
[CH2:21]=[CH:22][C:23]#[N:24].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[cH:9][c:10]([CH:11]=[CH:12][c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[Cl:19])[nH:20]2>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[cH:9][c:10](/[CH:11]=[CH:12]/[c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[Cl:19])[n:20]2[CH2:21][CH2:22...
C=CC#N.COc1ccc2[nH]c(C=Cc3ccccc3Cl)cc2c1
COc1ccc2c(c1)cc(/C=C/c1ccccc1Cl)n2CCC#N
null
N12CCCCCC2=NCCC1
O.C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
dbe06308fd0a5047c92f3bac96d8c1a8251ac4669b293e46c18abb750e9b5de1
9a626e72af92b4926e3e632773bc972f63cd9f1cf5e0e294f2aa92f80c10ca13
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
[CH2;D1;+0:1]=[CH;D2;+0:2]-[C:3]#[N;D1;H0:4].[c:5]-[C:6]=[C:7]-[c:8]1:[c:9]:[c:10]:[c:11](:[c:12]):[nH;D2;+0:13]:1>>[N;D1;H0:4]#[C:3]-[CH2;D2;+0:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:13]1:[c:8](/[C:7]=[C:6]/[c:5]):[c:9]:[c:10]:[c:11]:1:[c:12]
77
[{"value": 77.0, "product": "ClC1=C(C=CC=C1)/C=C/C=1N(C2=CC=C(C=C2C1)OC)CCC#N", "details": "PERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
To a solution of trans-diene (27) prepared as described in example 37 (1.5 g, 5.25 mmol) in acetonitrile (30 mL) was added acrylonitrile (2.42 mL, 36.8 mmol) and 1,8-diazabicyclo[5,4,0]undec-7-ene (20 drops). The resulting solution was stirred at room temperature under nitrogen for 18 h before being diluted with water ...
10.6084/m9.figshare.5104873.v1
null
Vinyl
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
null
N12CCCCCC2=NCCC1.O.C(C)#N
null
18
C=CC#N.COc1ccc2[nH]c(C=Cc3ccccc3Cl)cc2c1>N12CCCCCC2=NCCC1.O.C(C)#N>COc1ccc2c(c1)cc(/C=C/c1ccccc1Cl)n2CCC#N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8450601e0b244db8a4f671e080a931b1
COc1ccc2c(c1)cc(/C=C/c1ccccc1Cl)n2CCC#N.O=C1C=CC(=O)N1>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC#N)C(=O)NC3=O
ClC1=C(C=CC=C1)/C=C/C=1N(C2=CC=C(C=C2C1)OC)CCC#N.C1(C=CC(N1)=O)=O>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC#N
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[cH:9][c:21](/[CH:20]=[CH:12]/[c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[Cl:19])[n:22]2[CH2:23][CH2:24][C:25]#[N:26].[CH:10]1=[CH:11][C:27](=[O:28])[NH:29][C:30]1=[O:31]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[c:9]1[c:10]3[c:11]([c:12](-[c:13]4[cH:14][cH:15]...
COc1ccc2c(c1)cc(/C=C/c1ccccc1Cl)n2CCC#N.O=C1C=CC(=O)N1
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC#N)C(=O)NC3=O
null
null
null
Miscellaneous
OtherReaction
06ebd2a4d1c4338655a13edf4585639bd7722f7dc8ca7be18dccccea69c13187
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
[C:1]-[#7;a:2]1:[c:3](/[CH;D2;+0:4]=[CH;D2;+0:5]/[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](-[Cl;D1;H0:10]):[c:11]):[cH;D2;+0:12]:[c:13](:[c:14]):[c:15]:1:[c:16].[O;D1;H0:17]=[C:18]1-[#7:19]-[C:20](=[O;D1;H0:21])-[CH;D2;+0:22]=[CH;D2;+0:23]-1>>[C:1]-[#7;a:2]1:[c:3]2:[cH;D2;+0:4]:[c;H0;D3;+0:5](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:...
80.2
[{"value": 80.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 80.2, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Diene (236) (1.30 g, 3.86 mmol) prepared as described in example 96 was reacted with maleimide (0.49 g) following The procedure described in example 68 and then aromatized according to the procedure described in example 70 to give crude material that was chromatographed on silica eluting with ethyl acetate/hexane (1:1)...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2[nH]ccc2c1.C1=CCNC1
C1NCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
null
null
null
null
COc1ccc2c(c1)cc(/C=C/c1ccccc1Cl)n2CCC#N.O=C1C=CC(=O)N1>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC#N)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ac8cb47f4c114e919ab994028c58afaa
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC#N)C(=O)NC3=O>>N#CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC#N>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC#N
C[O:10][c:9]1[cH:8][cH:7][c:6]2[n:5]([CH2:4][CH2:3][C:2]#[N:1])[c:25]3[c:13]([c:12]2[cH:11]1)[c:14]1[c:15]([c:16](-[c:17]2[cH:18][cH:19][cH:20][cH:21][c:22]2[Cl:23])[cH:24]3)[C:26](=[O:27])[NH:28][C:29]1=[O:30]>>[N:1]#[C:2][CH2:3][CH2:4][n:5]1[c:6]2[cH:7][cH:8][c:9]([OH:10])[cH:11][c:12]2[c:13]2[c:14]3[c:15]([c:16](-[c...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC#N)C(=O)NC3=O
N#CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
null
null
CO
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
89.3
[{"value": 89.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.3, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Demethylation of nitrile (237) (0.15 g, 0.35 mmol) prepared as described in example 97 employing The procedure described in example 80, followed by trituration from methanol, gave phenol (238) (0.13 g, 89%) as an orange/yellow powder, mp 332–336° C. 1H NMR δ [(CD3)2SO] 11.10 (br s, 1H), 9.42 (br s, 1H), 8.39 (d, J=2.4 ...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
CO
null
null
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC#N)C(=O)NC3=O>CO>N#CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-60c9c68580eb4ab0aadc7efe56b5175a
Cc1c(Cl)cccc1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>Clc1cccc(Cl)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.ClC1=C(C(=CC=C1)Cl)C.BrN1C(CCC1=O)=O>>[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1)Cl
[Cl:1][c:2]1[cH:3][cH:4][cH:5][c:6]([Cl:7])[c:8]1[CH3:9].O=C1CCC(=O)N1[Br:29].[P:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[Cl:1][c:2]1[cH:3][cH:4][cH:5][c:6]([Cl:7])[c:8]1[CH2:9][P+:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][c...
Cc1c(Cl)cccc1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1
Clc1cccc(Cl)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
null
N(=NC(C#N)(C)C)C(C#N)(C)C
C1=CC=CC=C1
Miscellaneous
OtherReaction
90798389381727105f8f2fc21b48c935111a22021515f706338ce609a905e694
7953bead7af5583757c739601734838d384eb4a189267c5eeec33f580917362a
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:1].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
99
[{"value": 99.0, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.9, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 2,6-dichlorotoluene (20.1 g, 0.125 mol), N-bromosuccinimide (24.6 g, 0.138 mol) and 2,2′-azobisisobutyronitrile (0.41 g, 2.50 mmol) in dry benzene (300 mL) under N2 was stirred at reflux for 6 h with continuous irradiation from a 100W lamp. The resulting reaction mixture was concentrated under vacuum (to 5...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
null
C1CCNC1
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
N(=NC(C#N)(C)C)C(C#N)(C)C.C1=CC=CC=C1
null
null
Cc1c(Cl)cccc1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>N(=NC(C#N)(C)C)C(C#N)(C)C.C1=CC=CC=C1>Clc1cccc(Cl)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-09c9625c2f0844eb972125fd587329d8
COc1ccc2[nH]c(C=O)cc2c1.Clc1cccc(Cl)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1>>COc1ccc2[nH]c(/C=C/c3c(Cl)cccc3Cl)cc2c1
COC=1C=C2C=C(NC2=CC1)C=O.[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1)Cl.[Li+].CC(C)[N-]C(C)C>>ClC1=C(C(=CC=C1)Cl)/C=C/C=1NC2=CC=C(C=C2C1)OC
O=[CH:9][c:8]1[nH:7][c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:21][c:20]2[cH:19]1.c1ccc([P+](c2ccccc2)(c2ccccc2)[CH2:10][c:11]2[c:12]([Cl:13])[cH:14][cH:15][cH:16][c:17]2[Cl:18])cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[c:12]([Cl:13])[cH:14][cH:15][cH:16][c:17]3[Cl:18])[cH:19][c:20]2[cH...
COc1ccc2[nH]c(C=O)cc2c1.Clc1cccc(Cl)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1
COc1ccc2[nH]c(/C=C/c3c(Cl)cccc3Cl)cc2c1
null
null
null
C-C Coupling
Wittig with Phosphonium
cb5f277ac55a0e763ef643becc05f1522019cc4161daceb249ed2d634b78153b
cedc9d4b791e43eacf8e7ecfa6a98d1dc0438794e96e4f1c4bef436b78f82bd8
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[c:6]:[c:7](-[CH2;D2;+0:8]-[P+](-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:9]>>[c:6]:[c:7](/[CH;D2;+0:8]=[CH;D2;+0:1]/[c:2](:[c:3]):[#7;a:4]:[c:5]):[c:9]
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (O) was reacted with (2,6-dichlorobenzyl)(triphenyl)phosphonium bromide (511) prepared as described in example 102 using the procedure described in example 37, except that the LDA and aldehyde were (sequentially) added at 0° C., the ratio of LDA aldehyde was 1.37:1 and the reactio...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
null
c1ccccc1.c1ccccc1.c1ccccc1
null
c1ccc2[nH]ccc2c1.c1ccccc1
HO-
null
null
5
COc1ccc2[nH]c(C=O)cc2c1.Clc1cccc(Cl)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1>>COc1ccc2[nH]c(/C=C/c3c(Cl)cccc3Cl)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-62d61bd7e7f844569eafefc807ca8df6
Cc1c(Br)cccc1Br.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>Brc1cccc(Br)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
BrC1=C(C(=CC=C1)Br)C.C1CC(=O)N(C1=O)Br.CC(C)(C#N)N=NC(C)(C)C#N.[Br-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].BrC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1)Br
[Br:1][c:2]1[cH:3][cH:4][cH:5][c:6]([Br:7])[c:8]1[CH3:9].O=C1CCC(=O)N1[Br:29].[P:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[Br:1][c:2]1[cH:3][cH:4][cH:5][c:6]([Br:7])[c:8]1[CH2:9][P+:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][c...
Cc1c(Br)cccc1Br.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1
Brc1cccc(Br)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
null
null
C(Cl)Cl.C1=CC=CC=C1
Miscellaneous
OtherReaction
90798389381727105f8f2fc21b48c935111a22021515f706338ce609a905e694
7953bead7af5583757c739601734838d384eb4a189267c5eeec33f580917362a
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:1].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
95
[{"value": 95.0, "product": "[Br-].BrC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1)Br", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
Bromination of 2,6-dibromotoluene with NBS/AIBN, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 102, except that the reaction time for the bromination was 3 h, gave the phosphonium salt (516) (95%) as a cream powder, mp (CH2Cl2/benzene) 241–243° C. 1H NMR (CD...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
null
C1CCNC1
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(Cl)Cl.C1=CC=CC=C1
null
3
Cc1c(Br)cccc1Br.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C(Cl)Cl.C1=CC=CC=C1>Brc1cccc(Br)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-59650bb3fb5849e1898bd638217fd9f7
Brc1cccc(Br)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc2[nH]c(/C=C/c3c(Br)cccc3Br)cc2c1
OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].BrC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1)Br.[Li+].CC(C)[N-]C(C)C>>BrC1=C(C(=CC=C1)Br)/C=C/C=1NC2=CC=C(C=C2C1)OC
c1ccc([P+](c2ccccc2)(c2cccc[cH:1]2)[CH2:10][c:11]2[c:12]([Br:13])[cH:14][cH:15][cH:16][c:17]2[Br:18])cc1.O=C1NC(=O)c2c1c(I)[cH:9][c:8]1[nH:7][c:6]3[cH:5][cH:4][c:3]([OH:2])[cH:21][c:20]3[c:19]21>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[c:12]([Br:13])[cH:14][cH:15][cH:16][c:17]3[Br:18])[c...
Brc1cccc(Br)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21
COc1ccc2[nH]c(/C=C/c3c(Br)cccc3Br)cc2c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:[cH;D2;+0:15]:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:15]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[C...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2,6-dibromobenzyl)(triphenyl)phosphonium bromide (516) prepared as described in example 107 using the procedure described in example 37, except that the ratio of LDA:aldehyde was 1.37:1 and the reaction time was 5 h, to give (after crystallisation from CH2Cl2...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccccc1.c1ccccc1.c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
HI
null
null
5
Brc1cccc(Br)c1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc2[nH]c(/C=C/c3c(Br)cccc3Br)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e43bb02ecf6b45f3a5d7445a8e13c68c
Br.COc1cc(Cl)c(CO)c(Cl)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>COc1cc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
ClC1=C(C(=CC(=C1)OC)Cl)CO.Br.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC(=C1)OC)Cl
[BrH:31].O[CH2:8][c:7]1[c:5]([Cl:6])[cH:4][c:3]([O:2][CH3:1])[cH:30][c:28]1[Cl:29].[P:9]([c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)([c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1)[c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([Cl:6])[c:7]([CH2:8][P+:9]([c:10]2[cH:11][cH:12][cH:13][cH:14][cH:1...
Br.COc1cc(Cl)c(CO)c(Cl)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1
COc1cc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
null
null
C(C)(=O)O.C1=CC=CC=C1
Functional Group Interconversion
OtherReaction
bbb792e2dbaac6137f4ab4b2ad2edf8b90c54de5f7db3b319a5444b78b4405dc
5700379a096deb40e2dc50b293f55a01cfe36aa58cf97bdfa006d0b7ff21038e
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[BrH;D0;+0:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:5].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
100
[{"value": 100.0, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC(=C1)OC)Cl", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of (2,6-dichloro-4-methoxyphenyl)methanol (3.00 g, 14.5 mmol) in 30% HBr in acetic acid (45 mL) was stirred at 20° C. for 3 h, then poured onto ice-water (120 mL) and extracted with pentane (6×100 mL). The extracts were washed with water (3×200 mL), backextracting with pentane (100 mL). Removal of the solven...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
null
null
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(C)(=O)O.C1=CC=CC=C1
null
null
Br.COc1cc(Cl)c(CO)c(Cl)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C(C)(=O)O.C1=CC=CC=C1>COc1cc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a5188ceed6ed4d199e64c5818e4ba7f6
COc1cc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1cc(Cl)c(/C=C/c2cc3cc(OC)ccc3[nH]2)c(Cl)c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC(=C1)OC)Cl>>ClC1=C(C(=CC(=C1)OC)Cl)/C=C/C=1NC2=CC=C(C=C2C1)OC
c1ccc([P+](c2ccccc2)(c2ccccc2)[CH2:8][c:7]2[c:5]([Cl:6])[cH:4][c:3]([O:2][CH3:1])[cH:23][c:21]2[Cl:22])cc1.O=C1NC(=O)c2c1c(I)[cH:9][c:10]1[c:11]2[c:12]2[cH:13][c:14]([OH:15])[cH:17][cH:18][c:19]2[nH:20]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([Cl:6])[c:7](/[CH:8]=[CH:9]/[c:10]2[cH:11][c:12]3[cH:13][c:14]([O:15][CH3:16])[cH:17]...
COc1cc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21
COc1cc(Cl)c(/C=C/c2cc3cc(OC)ccc3[nH]2)c(Cl)c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:15]>>[C;D1;H3:16]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[CH;D2;+0:14]/[c...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2,6-dichloro-4-methoxybenzyl)(triphenyl)phosphonium bromide (521), prepared as described in example 112, using the procedure described in example 37, except that the aldehyde was added at 0° C., the ratio of LDA:aldehyde was 1.37:1 and the reaction time was 5...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccccc1.c1ccccc1.c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3
c1ccc2[nH]ccc2c1
c1ccccc1.c1ccc2[nH]ccc2c1
HI
null
null
5
COc1cc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1cc(Cl)c(/C=C/c2cc3cc(OC)ccc3[nH]2)c(Cl)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-45cd2ce8b12c4a538ef3a33a64d2aec4
Br.COc1ccc(Cl)c(CO)c1Cl.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.[Br-]
ClC1=C(C(=CC=C1OC)Cl)CO.Br.[Br-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1OC)Cl
[BrH:31].O[CH2:9][c:8]1[c:6]([Cl:7])[cH:5][cH:4][c:3]([O:2][CH3:1])[c:29]1[Cl:30].[P:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[c:8]([CH2:9][P+:10]([c:11]2[cH:12][cH:13][cH:14][cH:1...
Br.COc1ccc(Cl)c(CO)c1Cl.c1ccc(P(c2ccccc2)c2ccccc2)cc1
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.[Br-]
null
null
C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1
Functional Group Interconversion
OtherReaction
bbb792e2dbaac6137f4ab4b2ad2edf8b90c54de5f7db3b319a5444b78b4405dc
5700379a096deb40e2dc50b293f55a01cfe36aa58cf97bdfa006d0b7ff21038e
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[BrH;D0;+0:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:5].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
97
[{"value": 97.0, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1OC)Cl", "details": "PERCENTYIELD", "is_desired": false}]
null
null
36
HOUR
Bromination of (2,6-dichloro-3-methoxyphenyl)methanol with 30% HBr in acetic acid, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 112, except that the reaction time for the displacement was 36 h, gave the phosphonium salt (526) (97%) as a white solid, mp (CH2...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
null
null
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1
null
36
Br.COc1ccc(Cl)c(CO)c1Cl.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1>COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b68878edc0094592bc98e8d4a7c9806f
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc2[nH]c(/C=C/c3c(Cl)ccc(OC)c3Cl)cc2c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C(=CC=C1OC)Cl>>ClC1=C(C(=CC=C1OC)Cl)/C=C/C=1NC2=CC=C(C=C2C1)OC
c1ccc([P+](c2ccccc2)(c2cccc[cH:1]2)[CH2:10][c:11]2[c:12]([Cl:13])[cH:14][cH:15][c:16]([O:17][CH3:18])[c:19]2[Cl:20])cc1.O=C1NC(=O)c2c1c(I)[cH:9][c:8]1[nH:7][c:6]3[cH:5][cH:4][c:3]([OH:2])[cH:23][c:22]3[c:21]21>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[c:12]([Cl:13])[cH:14][cH:15][c:16]([O...
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21
COc1ccc2[nH]c(/C=C/c3c(Cl)ccc(OC)c3Cl)cc2c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:[cH;D2;+0:15]:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:15]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[C...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2,6-dichloro-3-methoxybenzyl)(triphenyl)phosphonium bromide (526), prepared as described in example 117, using the procedure described in example 37, except that the aldehyde was added at 0° C., the ratio of LDA:aldehyde was 1.55:1 and the reaction time was 5...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccccc1.c1ccccc1.c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
HI
null
null
5
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc2[nH]c(/C=C/c3c(Cl)ccc(OC)c3Cl)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1db8bc6974f04497a060aa2801e1f53f
Brc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc2[nH]c(/C=C/c3ccccc3Br)cc2c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].BrC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC=C1>>BrC1=C(C=CC=C1)/C=C/C=1NC2=CC=C(C=C2C1)OC
c1ccc([P+](c2ccccc2)(c2cccc[cH:1]2)[CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[Br:17])cc1.O=C1NC(=O)c2c1c(I)[cH:9][c:8]1[nH:7][c:6]3[cH:5][cH:4][c:3]([OH:2])[cH:20][c:19]3[c:18]21>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[Br:17])[cH:18][c:19]2[cH:...
Brc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21
COc1ccc2[nH]c(/C=C/c3ccccc3Br)cc2c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:[cH;D2;+0:15]:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:15]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[C...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2-bromobenzyl)(triphenyl)phosphonium bromide using the procedure described in example 37, except that the aldehyde was added at 0° C., the ratio of LDA:aldehyde was 1.46:1 and the reaction time was 5 h, to give (after crystallisation from CH2Cl2/hexane) the d...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccccc1.c1ccccc1.c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
HI
null
null
5
Brc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc2[nH]c(/C=C/c3ccccc3Br)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9657ba143e4645cb9448f995c724a097
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1>>COc1ccc2[nH]c(/C=C/c3ccccc3[N+](=O)[O-])cc2c1
OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Cl-].[N+](=O)([O-])C1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC=C1.[Li+].CC(C)[N-]C(C)C>>COC=1C=C2C=C(NC2=CC1)\C=C\C1=C(C=CC=C1)[N+](=O)[O-]
O=C1N[C:1](=O)c2c(I)[cH:9][c:8]3[nH:7][c:6]4[cH:5][cH:4][c:3]([OH:2])[cH:22][c:21]4[c:20]3c21.c1ccc([P+](c2ccccc2)(c2ccccc2)[CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[N+:17](=[O:18])[O-:19])cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[N+:17](=[O...
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1
COc1ccc2[nH]c(/C=C/c3ccccc3[N+](=O)[O-])cc2c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-[C;H0;D3;+0:12](=O)-N-C-2=O.[c:13]:[c:14](-[CH2;D2;+0:15]-[P+](-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:12]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2-nitrobenzyl)(triphenyl)phosphonium chloride using the procedure described in example 37, except that the ratio of LDA:aldehyde was 1.37:1 and the reaction time was 5 h, to give (after crystallisation from CH2Cl2/hexane) the diene (536) as red-orange crystal...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccc2c(c1)nc1ccc3c(c12)CNC3.c1ccccc1.c1ccccc1.c1ccccc1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
HI
null
null
5
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1>>COc1ccc2[nH]c(/C=C/c3ccccc3[N+](=O)[O-])cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a45e48d54ee2440894b7512541d2c34c
Cc1ccccc1C#N.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>N#Cc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
C=1(C(=CC=CC1)C#N)C.C1CC(=O)N(C1=O)Br.CC(C)(C#N)N=NC(C)(C)C#N.[Br-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].C(#N)C1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC=C1
[N:1]#[C:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[CH3:9].O=C1CCC(=O)N1[Br:29].[P:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[N:1]#[C:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[CH2:9][P+:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16...
Cc1ccccc1C#N.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1
N#Cc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
null
null
C(Cl)Cl.C1=CC=CC=C1
Miscellaneous
OtherReaction
90798389381727105f8f2fc21b48c935111a22021515f706338ce609a905e694
7953bead7af5583757c739601734838d384eb4a189267c5eeec33f580917362a
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:1].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
70
[{"value": 70.0, "product": "[Br-].C(#N)C1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
Bromination of o-tolunitrile with NBS/AIBN, followed by reaction of the crude bromide with triphenylphosphine (1.2 equiv.), using the procedure described in example 102, except that the reaction time for the bromination was 2 h, gave the phosphonium salt (547) (70%) as a light brown powder, mp (CH2Cl2/benzene) 237–241°...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
null
C1CCNC1
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(Cl)Cl.C1=CC=CC=C1
null
2
Cc1ccccc1C#N.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C(Cl)Cl.C1=CC=CC=C1>N#Cc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a392b1c912f748078ea5ee9702ba2f24
N#Cc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc2[nH]c(/C=C/c3ccccc3C#N)cc2c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].C(#N)C1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC=C1.[Li+].CC(C)[N-]C(C)C>>COC=1C=C2C=C(NC2=CC1)/C=C/C1=C(C#N)C=CC=C1
c1ccc([P+](c2ccccc2)(c2cccc[cH:1]2)[CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[C:17]#[N:18])cc1.O=C1NC(=O)c2c1c(I)[cH:9][c:8]1[nH:7][c:6]3[cH:5][cH:4][c:3]([OH:2])[cH:21][c:20]3[c:19]21>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[C:17]#[N:18])[cH:19...
N#Cc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21
COc1ccc2[nH]c(/C=C/c3ccccc3C#N)cc2c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:[cH;D2;+0:15]:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:15]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[C...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2-cyanobenzyl)(triphenyl)phosphonium bromide (547) prepared as described in example 136 using the procedure described in example 37, except that the LDA and aldehyde were (sequentially) added at 0° C., the ratio of LDA:aldehyde was 1.55:1 and the reaction tim...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccccc1.c1ccccc1.c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
HI
null
null
5
N#Cc1ccccc1C[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc2[nH]c(/C=C/c3ccccc3C#N)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2712ded50a36435682981de16c8069c0
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1>>COc1ccc2[nH]c(/C=C/c3cccc([N+](=O)[O-])c3)cc2c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].[N+](=O)([O-])C=1C=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC1.[Li+].CC(C)[N-]C(C)C>>COC=1C=C2C=C(NC2=CC1)\C=C\C1=CC(=CC=C1)[N+](=O)[O-]
O=C1NC(=O)c2c1c(I)[cH:9][c:8]1[nH:7][c:6]3[cH:5][cH:4][c:3]([OH:2])[cH:22][c:21]3[c:20]21.c1ccc([P+](c2ccccc2)(c2cccc[cH:1]2)[CH2:10][c:11]2[cH:12][cH:13][cH:14][c:15]([N+:16](=[O:17])[O-:18])[cH:19]2)cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[cH:12][cH:13][cH:14][c:15]([N+:16](=[O:17]...
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1
COc1ccc2[nH]c(/C=C/c3cccc([N+](=O)[O-])c3)cc2c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:[cH;D2;+0:15]:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:15]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[C...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (3-nitrobenzyl)(triphenyl)phosphonium bromide using the procedure described in example 37, except that the LDA and aldehyde were sequentially added at 0° C., the ratio of LDA:aldehyde was 1.5:1 and the reaction time was 5 h, to give (after crystallisation from...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccc2c(c1)nc1ccc3c(c12)CNC3.c1ccccc1.c1ccccc1.c1ccccc1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
HI
null
null
5
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1>>COc1ccc2[nH]c(/C=C/c3cccc([N+](=O)[O-])c3)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fa1cddeabd1848c58bbff604171a8e90
Cc1cccc([N+](=O)[O-])c1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.[Br-]
ClC1=C(C=CC=C1[N+](=O)[O-])C.C1CC(=O)N(C1=O)Br.CC(C)(C#N)N=NC(C)(C)C#N.[Br-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC=C1[N+](=O)[O-]
[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][cH:7][c:8]([CH3:9])[c:29]1[Cl:30].O=C1CCC(=O)N1[Br:31].[P:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][cH:7][c:8]([CH2:9][P+:10]([c:11]2[cH:12][cH:13...
Cc1cccc([N+](=O)[O-])c1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1
O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.[Br-]
null
null
C(Cl)Cl.C1=CC=CC=C1
Miscellaneous
OtherReaction
90798389381727105f8f2fc21b48c935111a22021515f706338ce609a905e694
7953bead7af5583757c739601734838d384eb4a189267c5eeec33f580917362a
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:1].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
44
[{"value": 44.0, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC=C1[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
Bromination of 2-chloro-3-nitrotoluene with NBS/AIBN, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 102, except that the reaction time for the bromination was 2 h and the displacement reaction was performed at 70° C. for 1 d, gave the phosphonium salt (554) ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
null
C1CCNC1
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(Cl)Cl.C1=CC=CC=C1
null
2
Cc1cccc([N+](=O)[O-])c1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C(Cl)Cl.C1=CC=CC=C1>O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0a3ddf2f18b44842bcac40e66ad962e1
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl>>COc1ccc2[nH]c(/C=C/c3cccc([N+](=O)[O-])c3Cl)cc2c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC=C1[N+](=O)[O-].[Li+].CC(C)[N-]C(C)C>>ClC1=C(C=CC=C1[N+](=O)[O-])/C=C/C=1NC2=CC=C(C=C2C1)OC
O=C1NC(=O)c2c1c(I)[cH:9][c:8]1[nH:7][c:6]3[cH:5][cH:4][c:3]([OH:2])[cH:23][c:22]3[c:21]21.c1ccc([P+](c2ccccc2)(c2cccc[cH:1]2)[CH2:10][c:11]2[cH:12][cH:13][cH:14][c:15]([N+:16](=[O:17])[O-:18])[c:19]2[Cl:20])cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[cH:12][cH:13][cH:14][c:15]([N+:16](=...
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl
COc1ccc2[nH]c(/C=C/c3cccc([N+](=O)[O-])c3Cl)cc2c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:[cH;D2;+0:15]:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:15]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[C...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2-chloro-3-nitrobenzyl)(triphenyl)phosphonium bromide (554) preared as described in example 143 using the procedure described in example 37, except that the LDA and aldehyde were (sequentially) added at 0° C., the ratio of LDA:aldehyde was 1.5:1 and the react...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccc2c(c1)nc1ccc3c(c12)CNC3.c1ccccc1.c1ccccc1.c1ccccc1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
HI
null
null
5
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1cccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1Cl>>COc1ccc2[nH]c(/C=C/c3cccc([N+](=O)[O-])c3Cl)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b77c515b4e7647afacc2b1635151178a
Cc1ccc([N+](=O)[O-])cc1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>O=[N+]([O-])c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
ClC1=C(C=CC(=C1)[N+](=O)[O-])C.C1CC(=O)N(C1=O)Br.CC(C)(C#N)N=NC(C)(C)C#N.[Br-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC(=C1)[N+](=O)[O-]
[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([CH3:8])[c:28]([Cl:29])[cH:30]1.O=C1CCC(=O)N1[Br:31].[P:9]([c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)([c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1)[c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([CH2:8][P+:9]([c:10]2[cH:11][cH:12][cH:...
Cc1ccc([N+](=O)[O-])cc1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1
O=[N+]([O-])c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
null
null
C1=CC=CC=C1
Miscellaneous
OtherReaction
90798389381727105f8f2fc21b48c935111a22021515f706338ce609a905e694
7953bead7af5583757c739601734838d384eb4a189267c5eeec33f580917362a
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:1].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
34
[{"value": 34.0, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC(=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
Bromination of 2-chloro-4-nitrotoluene with NBS/AIBN, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 102, except that the reaction time for the bromination was 24 h and the displacement reaction was performed at 20° C. for 7 d, gave the crude phosphonium salt...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
null
C1CCNC1
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C1=CC=CC=C1
null
24
Cc1ccc([N+](=O)[O-])cc1Cl.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C1=CC=CC=C1>O=[N+]([O-])c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d71f862c74a843f7a18c5255b186b546
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1>>COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Cl)cc2c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC(=C1)[N+](=O)[O-].[Li+].CC(C)[N-]C(C)C>>ClC1=C(C=CC(=C1)[N+](=O)[O-])/C=C/C=1NC2=CC=C(C=C2C1)OC
O=C1NC(=O)c2c1c(I)[cH:9][c:8]1[nH:7][c:6]3[cH:5][cH:4][c:3]([OH:2])[cH:23][c:22]3[c:21]21.c1ccc([P+](c2ccccc2)(c2cccc[cH:1]2)[CH2:10][c:11]2[cH:12][cH:13][c:14]([N+:15](=[O:16])[O-:17])[cH:18][c:19]2[Cl:20])cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8](/[CH:9]=[CH:10]/[c:11]3[cH:12][cH:13][c:14]([N+:15](=[O:16])...
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1
COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Cl)cc2c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:[cH;D2;+0:15]:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:15]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[C...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2-chloro-4-nitrobenzyl)(triphenyl)phosphonium bromide (559) prepared as described in example 148 using the procedure described in example 37, except that the LDA and aldehyde were (sequentially) added at 0° C., the ratio of LDA:aldehyde was 1.5:1 and the reac...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccc2c(c1)nc1ccc3c(c12)CNC3.c1ccccc1.c1ccccc1.c1ccccc1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
HI
null
null
5
O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21.O=[N+]([O-])c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1>>COc1ccc2[nH]c(/C=C/c3ccc([N+](=O)[O-])cc3Cl)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5ff65fcfe3074652ab6aafbfe9be302d
Br.O=[N+]([O-])c1ccc(Cl)c(CO)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>O=[N+]([O-])c1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.[Br-]
ClC1=C(C=C(C=C1)[N+](=O)[O-])CO.Br.[Br-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=C(C=C1)[N+](=O)[O-]
[BrH:31].O[CH2:10][c:9]1[c:7]([Cl:8])[cH:6][cH:5][c:4]([N+:2](=[O:1])[O-:3])[cH:30]1.[P:11]([c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1)([c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1)[c:24]1[cH:25][cH:26][cH:27][cH:28][cH:29]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([Cl:8])[c:9]([CH2:10][P+:11]([c:12]2[cH:13][cH:14]...
Br.O=[N+]([O-])c1ccc(Cl)c(CO)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1
O=[N+]([O-])c1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.[Br-]
null
null
C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1
Functional Group Interconversion
OtherReaction
bbb792e2dbaac6137f4ab4b2ad2edf8b90c54de5f7db3b319a5444b78b4405dc
5700379a096deb40e2dc50b293f55a01cfe36aa58cf97bdfa006d0b7ff21038e
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[BrH;D0;+0:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:5].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
63
[{"value": 63.0, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=C(C=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Bromination of (2-chloro-5-nitrophenyl)methanol with 30% HBr in acetic acid, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 112, gave the phosphonium salt (564) (63%) as a white solid, mp (CH2Cl2/benzene) 239–243° C. 1H NMR (CDCl3) δ 8.22 (br s, 1H), 8.07 (br...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
null
null
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1
null
null
Br.O=[N+]([O-])c1ccc(Cl)c(CO)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1>O=[N+]([O-])c1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b0cc435ca11b4dacb9b6522a9e461fa6
Br.COc1ccc(CO)c(Cl)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>COc1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
ClC1=C(C=CC(=C1)OC)CO.Br.[Br-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC(=C1)OC
[BrH:30].O[CH2:7][c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:29][c:27]1[Cl:28].[P:8]([c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)([c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1)[c:21]1[cH:22][cH:23][cH:24][cH:25][cH:26]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][P+:8]([c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)([c:15]2[cH:...
Br.COc1ccc(CO)c(Cl)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1
COc1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
null
null
C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1
Functional Group Interconversion
OtherReaction
bbb792e2dbaac6137f4ab4b2ad2edf8b90c54de5f7db3b319a5444b78b4405dc
5700379a096deb40e2dc50b293f55a01cfe36aa58cf97bdfa006d0b7ff21038e
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[BrH;D0;+0:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:5].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
100
[{"value": 100.0, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC(=C1)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
Bromination of (2-chloro-4-methoxyphenyl)methanol with 30% HBr in acetic acid, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 112, except that the reaction time for the bromination was 4 h and the reaction time for the displacement was 28 h, gave the phosphon...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
null
null
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1
null
4
Br.COc1ccc(CO)c(Cl)c1.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C(C)(=O)O.C(Cl)Cl.C1=CC=CC=C1>COc1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7ccdd8dbcf034a15acfdf0ca50cc01a9
COc1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc(/C=C/c2cc3cc(OC)ccc3[nH]2)c(Cl)c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC(=C1)OC.[Li+].CC(C)[N-]C(C)C>>ClC1=C(C=CC(=C1)OC)/C=C/C=1NC2=CC=C(C=C2C1)OC
c1ccc([P+](c2ccccc2)(c2cccc[cH:15]2)[CH2:7][c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:22][c:20]2[Cl:21])cc1.O=C1NC(=O)c2c1c(I)[cH:8][c:9]1[c:10]2[c:11]2[cH:12][c:13]([OH:14])[cH:16][cH:17][c:18]2[nH:19]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](/[CH:7]=[CH:8]/[c:9]2[cH:10][c:11]3[cH:12][c:13]([O:14][CH3:15])[cH:16][cH:17][c:...
COc1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21
COc1ccc(/C=C/c2cc3cc(OC)ccc3[nH]2)c(Cl)c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:[cH;D2;+0:15]:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:16]>>[CH3;D1;+0:15]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[C...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2-chloro-4-methoxybenzyl)(triphenyl)phosphonium bromide (574) prepared as described in example 162 using the procedure described in example 37, except that the LDA and aldehyde were sequentially added at 0° C., the ratio of LDA:aldehyde was 1.5:1 and the reac...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccccc1.c1ccccc1.c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3
c1ccc2[nH]ccc2c1
c1ccccc1.c1ccc2[nH]ccc2c1
HI
null
null
5
COc1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c(Cl)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc(/C=C/c2cc3cc(OC)ccc3[nH]2)c(Cl)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bfdc92081d604501937dbab0c74fb0e9
COc1ccc(Cl)c(C)c1.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.[Br-]
ClC1=C(C=C(C=C1)OC)C.C1CC(=O)N(C1=O)Br.CC(C)(C#N)N=NC(C)(C)C#N.[Br-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=C(C=C1)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[c:8]([CH3:9])[cH:29]1.O=C1CCC(=O)N1[Br:30].[P:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[c:8]([CH2:9][P+:10]([c:11]2[cH:12][cH:13][cH:14]...
COc1ccc(Cl)c(C)c1.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.[Br-]
null
null
C(Cl)Cl.C1=CC=CC=C1
Miscellaneous
OtherReaction
90798389381727105f8f2fc21b48c935111a22021515f706338ce609a905e694
7953bead7af5583757c739601734838d384eb4a189267c5eeec33f580917362a
c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5].[c:6]:[c:7](-[P;H0;D3;+0:8](-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]>>[Br-;H0;D0:1].[c:6]:[c:7](-[P+;H0;D4:8](-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5])(-[c:9](:[c:10]):[c:11])-[c:12](:[c:13]):[c:14]):[c:15]
76
[{"value": 76.0, "product": "[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=C(C=C1)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
Bromination of 1-chloro-4-methoxy-2-methylbenzene with NBS/AIBN, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 102, except that the reaction time for the bromination was 4 h, gave the phosphonium salt (578) (76%) as a light brown solid, mp (CH2Cl2/benzene) 1...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
null
C1CCNC1
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(Cl)Cl.C1=CC=CC=C1
null
4
COc1ccc(Cl)c(C)c1.O=C1CCC(=O)N1Br.c1ccc(P(c2ccccc2)c2ccccc2)cc1>C(Cl)Cl.C1=CC=CC=C1>COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.[Br-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-75df05aa2dc442c2a14c9e3dbed3c708
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc(Cl)c(/C=C/c2cc3cc(OC)ccc3[nH]2)c1
[Li+].CC(C)[N-]C(C)C.OC1=CC=2C=3C4=C(C(=CC3NC2C=C1)I)C(NC4=O)=O.[Br-].ClC1=C(C[P+](C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=C(C=C1)OC.[Li+].CC(C)[N-]C(C)C>>ClC1=C(C=C(C=C1)OC)/C=C/C=1NC2=CC=C(C=C2C1)OC
c1ccc([P+](c2ccccc2)(c2ccccc2)[CH2:9][c:8]2[c:6]([Cl:7])[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:22]2)cc1.O=C1NC(=O)c2c1c(I)[cH:10][c:11]1[c:12]2[c:13]2[cH:14][c:15]([OH:16])[cH:18][cH:19][c:20]2[nH:21]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[c:8](/[CH:9]=[CH:10]/[c:11]2[cH:12][c:13]3[cH:14][c:15]([O:16][CH3:17])[cH:18...
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21
COc1ccc(Cl)c(/C=C/c2cc3cc(OC)ccc3[nH]2)c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
76e526426ecd806adac24971ec22abcee22f8ef37d02feb5b78b4790d43dc040
298bbddbbad66b4d8f09c0f74d9ca58c3f96284e4a5a7f4c53c37cace7b0e319
C(=C/c1cc2ccccc2[nH]1)\c1ccccc1
I-c1:[cH;D2;+0:1]:[c:2]2:[#7;a:3]:[c:4]3:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10]:3:[c;H0;D3;+0:11]:2:c2:c:1-C(=O)-N-C-2=O.[c:12]:[c:13](-[CH2;D2;+0:14]-[P+](-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:15]>>[C;D1;H3:16]-[O;H0;D2;+0:8]-[c:7]1:[c:9]:[c:10]2:[cH;D2;+0:11]:[c:2](/[CH;D2;+0:1]=[CH;D2;+0:14]/[c...
null
[]
null
null
5
HOUR
The 5-methoxy-1H-indole-2-carbaldehyde (1) was reacted with (2-chloro-5-methoxybenzyl)(triphenyl)phosphonium bromide (578) prepared as described in example 166 using the procedure described in example 37, except that the LDA and aldehyde were (sequentially) added at 0° C., the ratio of LDA:aldehyde was 1.5:1 and the re...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Unsubstituted dicarboximide.Aromatic alcohol
Ether
c1ccccc1.c1ccccc1.c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3
c1ccc2[nH]ccc2c1
c1ccccc1.c1ccc2[nH]ccc2c1
HI
null
null
5
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.O=C1NC(=O)c2c1c(I)cc1[nH]c3ccc(O)cc3c21>>COc1ccc(Cl)c(/C=C/c2cc3cc(OC)ccc3[nH]2)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0f71807f4508467783c850c345328123
CNC.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>>CN(C)CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.Cl.C([O-])([O-])=O.[K+].[K+].CNC>>CN(CCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O)C
[CH3:1][NH:2][CH3:3].Br[CH2:4][CH2:5][CH2:6][n:7]1[c:8]2[cH:9][cH:10][c:11]([OH:12])[cH:13][c:14]2[c:15]2[c:16]3[c:17]([c:18](-[c:19]4[cH:20][cH:21][cH:22][cH:23][cH:24]4)[cH:25][c:26]12)[C:27](=[O:28])[NH:29][C:30]3=[O:31]>>[CH3:1][N:2]([CH3:3])[CH2:4][CH2:5][CH2:6][n:7]1[c:8]2[cH:9][cH:10][c:11]([OH:12])[cH:13][c:14]...
CNC.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr
CN(C)CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
null
null
CC(=O)N(C)C.O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
6d58cac08ccced0a33ed16fbca180bc12aa011288d6476106d98a7b2cbc3d709
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[C;D1;H3:4]-[NH;D2;+0:5]-[C;D1;H3:6]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:5](-[C;D1;H3:4])-[C;D1;H3:6]
47
[{"value": 47.0, "product": "CN(CCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O)C", "details": "PERCENTYIELD", "is_desired": false}]
80
CELSIUS
18
HOUR
To a solution of bromide (204) prepared as described in example 173 (0.12 g, 0.27 mmol) in dimethylacetamide (4 mL) was added the amine, dimethylamine (25 mol eq., 0.85 mL in this case as an 40% aqueous solution). The reaction vessel was sealed and heated at 80° C. with stirring for 18 h, before being diluted with wate...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
HBr
CC(=O)N(C)C.O
80
18
CNC.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>CC(=O)N(C)C.O>CN(C)CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c269c01594444c85b9e8d70f31ea4028
CNC.CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O>>CN(C)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
CS(=O)(=O)OCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.CNC>>CN(CCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O)C
[CH3:1][NH:2][CH3:3].CS(=O)(=O)O[CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[c:15]3[c:16]([c:17](-[c:18]4[cH:19][cH:20][cH:21][cH:22][cH:23]4)[cH:24][c:25]12)[C:26](=[O:27])[NH:28][C:29]3=[O:30]>>[CH3:1][N:2]([CH3:3])[CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]...
CNC.CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
CN(C)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
ba24696731c43f94422863463da0ee528bfb8ec715fd228fe0a6c2ae67b49c25
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[#7;a:3].[C;D1;H3:4]-[NH;D2;+0:5]-[C;D1;H3:6]>>[#7;a:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:5](-[C;D1;H3:4])-[C;D1;H3:6]
48
[{"value": 48.0, "product": "CN(CCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Mesylate (205) prepared as described in example 174 (70 mg, 0.16 mmol) was reacted with aqueous dimethylamine solution according to the procedure described in example 179 to give amine (209) (30 mg, 48%) as a yellow powder, mp 283–286° C. 1H NMR δ [(CD3)2SO] 11.05 (br s, 1H), 9.33 (s, 1H), 8.41 (d, J=2.4 Hz, 1H), 7.77 ...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
MsOH.HO-
null
null
null
CNC.CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O>>CN(C)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d4de17759f9b43b7a5dcf2c935b7db3d
C1COCCN1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCN1CCOCC1
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.N1CCOCC1>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCN1CCOCC1)C1=CC=CC=C1)C(NC4=O)=O
[NH:29]1[CH2:30][CH2:31][O:32][CH2:33][CH2:34]1.Br[CH2:28][CH2:27][CH2:26][n:25]1[c:16]2[cH:15][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)[c:7]3[c:6]([c:17]2[c:18]2[cH:19][c:20]([OH:21])[cH:22][cH:23][c:24]21)[C:4](=[O:5])[NH:3][C:2]3=[O:1]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11][...
C1COCCN1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCN1CCOCC1
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
2bad30dcdb0a20edb8ce877f072b133eedfd870621da393ec393128bfee00977
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCCN1CCOCC1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#8:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[#8:4]-[C:9]-[C:8]-1
72
[{"value": 72.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCN1CCOCC1)C1=CC=CC=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Bromide (204) (0.01 g, 0.22 mmol) prepared as described in example 173 was reacted with morpholine according to the procedure described in example 179 to give amine (210) (73 mg, 72%) as a yellow powder, mp 252–255° C. 1H NMR δ [(CD3)2SO] 11.04 (br s, 1H), 9.33 (s, 1H), 8.41 (d, J=2.5 Hz, 1H), 7.81 (s, 1H), 7.62 (m, 2H...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1COCCN1
C1COCC[NH]1
c1ccccc1.C1COCC[NH]1.C1NCc2c1ccc1nc3ccccc3c21
HBr
null
null
null
C1COCCN1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCN1CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d641bce625f5461193f6ee418249272a
C1COCCN1.CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCN1CCOCC1
CS(=O)(=O)OCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.N1CCOCC1>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCN1CCOCC1)C1=CC=CC=C1)C(NC4=O)=O
[NH:28]1[CH2:29][CH2:30][O:31][CH2:32][CH2:33]1.CS(=O)(=O)O[CH2:27][CH2:26][n:25]1[c:16]2[cH:15][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)[c:7]3[c:6]([c:17]2[c:18]2[cH:19][c:20]([OH:21])[cH:22][cH:23][c:24]21)[C:4](=[O:5])[NH:3][C:2]3=[O:1]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11]...
C1COCCN1.CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCN1CCOCC1
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
d65566d5f2049ef4dc70d5c480ea5af77518b25af8327af37e9d6d45c6baf558
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCN1CCOCC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[#7;a:3].[#8:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-1>>[#7;a:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[#8:4]-[C:9]-[C:8]-1
75
[{"value": 75.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCN1CCOCC1)C1=CC=CC=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Mesylate (205) (70 mg, 0.16 mmol) prepared as described in example 174 was reacted with morpholine according to the procedure described in example 179 to give amine (211) (53 mg, 75%) as a yellow powder, mp 260–262° C. 1H NMR □ [(CD3)2SO) 1H NMR δ [(CD3)2SO] 11.04 (br s, 1H), 9.33 (s, 1H), 8.40 (d, J=2.5 Hz, 1H), 7.78 ...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
C1COCCN1
C1COCC[NH]1
c1ccccc1.C1COCC[NH]1.C1NCc2c1ccc1nc3ccccc3c21
MsOH.HO-
null
null
null
C1COCCN1.CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCN1CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-99f392333f6a419c98f8fcb3e8e152c6
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr.c1c[nH]cn1>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCn1ccnc1
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.N1C=NC=C1>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCN1C=NC=C1)C1=CC=CC=C1)C(NC4=O)=O
Br[CH2:28][CH2:27][CH2:26][n:25]1[c:16]2[cH:15][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)[c:7]3[c:6]([c:17]2[c:18]2[cH:19][c:20]([OH:21])[cH:22][cH:23][c:24]21)[C:4](=[O:5])[NH:3][C:2]3=[O:1].[nH:29]1[cH:30][cH:31][n:32][cH:33]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11][cH:12][cH:1...
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr.c1c[nH]cn1
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCn1ccnc1
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
b9d84e1ee028da6e8c5d8924d45fbf8f3755d9adc2caf0035bd5ed7f30f5ee03
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCCn1ccnc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7;a:4]1:[c:5]:[c:6]:[nH;D2;+0:7]:[c:8]:1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:7]1:[c:6]:[c:5]:[#7;a:4]:[c:8]:1
53
[{"value": 53.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCN1C=NC=C1)C1=CC=CC=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Bromide (204) (80 mg, 0.18 mmol) prepared as described in example 173 was reacted with imidazole according to the procedure described in example 179 to give amine (212) (41 mg, 53%) as a yellow powder, mp 309–311° C. 1H NMR δ [(CD3)2SO] 11.06 (s, 1H), 9.36 (s, 1H), 8.40 (d, J=2.3 Hz, 1H), 7.69 (s, 1H), 7.64 (m, 3H), 7....
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1c[nH]cn1
c1c[nH]cn1
c1ccccc1.c1c[nH]cn1.C1NCc2c1ccc1nc3ccccc3c21
HBr
null
null
null
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr.c1c[nH]cn1>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCn1ccnc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-30442443bd474eb2884df4fb92dcbd48
CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O.c1c[nH]cn1>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCn1ccnc1
CS(=O)(=O)OCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.N1C=NC=C1>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCN1C=NC=C1)C1=CC=CC=C1)C(NC4=O)=O
CS(=O)(=O)O[CH2:27][CH2:26][n:25]1[c:16]2[cH:15][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)[c:7]3[c:6]([c:17]2[c:18]2[cH:19][c:20]([OH:21])[cH:22][cH:23][c:24]21)[C:4](=[O:5])[NH:3][C:2]3=[O:1].[nH:28]1[cH:29][cH:30][n:31][cH:32]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11][cH:12][cH:...
CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O.c1c[nH]cn1
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCn1ccnc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
c442140b096c54ef671e11ca8ca216d6e6322c408fe778838cc14d7f651c7f7d
0b4f3c8c88df0a792d0db7d59004d7fe5681a61dd48ef2449ddca2d636f76ada
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCn1ccnc1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[#7;a:3].[#7;a:4]1:[c:5]:[c:6]:[nH;D2;+0:7]:[c:8]:1>>[#7;a:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:7]1:[c:6]:[c:5]:[#7;a:4]:[c:8]:1
50
[{"value": 50.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCN1C=NC=C1)C1=CC=CC=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Mesylate (205) (70 mg, 0.16 mmol) prepared as described in example 174 was reacted with imidazole according to the procedure described in example 179 to give amine (213) (34 mg, 50%) as a yellow powder, mp>345° C. 1H NMR δ [(CD3)2SO] 11.05 (br s, 1H), 9.34 (s, 1H), 8.39 (d, J=2.4 Hz, 1H), 7.59 (m, 2H), 7.45 (m, 5H), 7....
10.6084/m9.figshare.5104873.v1
null
Mesylate
null
c1c[nH]cn1
c1c[nH]cn1
c1ccccc1.c1c[nH]cn1.C1NCc2c1ccc1nc3ccccc3c21
MsOH.HO-
null
null
null
CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O.c1c[nH]cn1>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCn1ccnc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bcc8870612fe4c60b84f7a1252511146
CN.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>>CNCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.CN>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCNC)C1=CC=CC=C1)C(NC4=O)=O
[CH3:1][NH2:2].Br[CH2:3][CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[c:15]3[c:16]([c:17](-[c:18]4[cH:19][cH:20][cH:21][cH:22][cH:23]4)[cH:24][c:25]12)[C:26](=[O:27])[NH:28][C:29]3=[O:30]>>[CH3:1][NH:2][CH2:3][CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[c:15]3[...
CN.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr
CNCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
null
null
CS(=O)C
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
fc19a1445ff204e66e51735d0191465bda3c6691fd233624a54742c9d4828411
0b1d32f56ad00f1e5bdae9390f9227bbea012fa2f8203aac34726b8a6761cc7c
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[C;D1;H3:4]-[NH2;D1;+0:5]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[NH;D2;+0:5]-[C;D1;H3:4]
61.2
[{"value": 61.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCNC)C1=CC=CC=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 61.2, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCNC)C1=CC=CC=C1)C(NC4=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Bromide (204) (40 mg, 0.09 mmol) prepared as described in example 173 was reacted with aqueous methylamine solution (10 mol equiv.) according to the procedure described in example 179 except that the reaction was performed in dimethylsulfoxide at room temperature for 3 h, to give amine (214) (22 mg, 61%) as an orange/y...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary amine
Secondary amine
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
HBr
CS(=O)C
null
null
CN.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>CS(=O)C>CNCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2a3230ac66084754a1ba89fe21f7b805
C1CNCCN1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCN1CCNCC1
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.N1CCNCC1>>OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCN1CCNCC1)C1=CC=CC=C1)C(NC4=O)=O
[NH:29]1[CH2:30][CH2:31][NH:32][CH2:33][CH2:34]1.Br[CH2:28][CH2:27][CH2:26][n:25]1[c:16]2[cH:15][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)[c:7]3[c:6]([c:17]2[c:18]2[cH:19][c:20]([OH:21])[cH:22][cH:23][c:24]21)[C:4](=[O:5])[NH:3][C:2]3=[O:1]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11]...
C1CNCCN1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCN1CCNCC1
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
61ec49e5207aa33ebff7094bb66b1d997d4af14524931a8b3643ef7a94219a9a
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCCN1CCNCC1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[#7:4]-[C:9]-[C:8]-1
55
[{"value": 55.0, "product": "OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCN1CCNCC1)C1=CC=CC=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
Bromide (204) (70 mg, 0.16 mmol) prepared as described in example 173 was reacted with piperazine according to The procedure described in example 179 except that the reaction was performed at room temperature for 20 h, to give amine (215) (40 mg, 55%) as a yellow powder, mp 178–183° C. 1H NMR δ [(CD3)2SO] 11.0 (br s, 1...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CNCCN1
C1C[NH]CCN1
c1ccccc1.C1C[NH]CCN1.C1NCc2c1ccc1nc3ccccc3c21
HBr
null
null
20
C1CNCCN1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCN1CCNCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-aece01f510ab41f1a3cba2126cfe5d57
Nc1ccccc1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCNc1ccccc1
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O.NC1=CC=CC=C1>>N(C1=CC=CC=C1)CCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O
[NH2:29][c:30]1[cH:31][cH:32][cH:33][cH:34][cH:35]1.Br[CH2:28][CH2:27][CH2:26][n:25]1[c:16]2[cH:15][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)[c:7]3[c:6]([c:17]2[c:18]2[cH:19][c:20]([OH:21])[cH:22][cH:23][c:24]21)[C:4](=[O:5])[NH:3][C:2]3=[O:1]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:...
Nc1ccccc1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCNc1ccccc1
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
fc19a1445ff204e66e51735d0191465bda3c6691fd233624a54742c9d4828411
0b1d32f56ad00f1e5bdae9390f9227bbea012fa2f8203aac34726b8a6761cc7c
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCCNc1ccccc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[NH;D2;+0:4]-[c:5](:[c:6]):[c:7]
38
[{"value": 38.0, "product": "N(C1=CC=CC=C1)CCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
Bromide (204) (75 mg, 0.17 mmol) prepared as described in example 173 was reacted with aniline according to the procedure described in example 179 except that the reaction was performed at room temperature for 20 h, to give aniline (217) (30 mg, 38%) as a yellow powder, mp 240° C. (dec). 1H NMR δ [(CD3)2SO] 11.04 (br s...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary amine
Secondary amine
null
null
c1ccccc1.c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
HBr
null
null
20
Nc1ccccc1.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCBr>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCNc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3891d5b333be4fc9af36bb80c85af3c7
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCBr.C[C@@H]1CNC[C@H](C)N1>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCN1C[C@@H](C)N[C@@H](C)C1
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1OC)Cl)C(NC3=O)=O)O.C[C@@H]1N[C@@H](CNC1)C>>ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCN2C[C@H](N[C@H](C2)C)C
Br[CH2:31][CH2:30][CH2:29][n:28]1[c:12]2[cH:11][c:10](-[c:9]3[c:3]([O:2][CH3:1])[cH:4][cH:5][cH:6][c:7]3[Cl:8])[c:15]3[c:14]([c:13]2[c:21]2[cH:22][c:23]([OH:24])[cH:25][cH:26][c:27]21)[C:19](=[O:20])[NH:18][C:16]3=[O:17].[NH:32]1[CH2:33][C@@H:34]([CH3:35])[NH:36][C@@H:37]([CH3:38])[CH2:39]1>>[CH3:1][O:2][c:3]1[cH:4][cH...
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCBr.C[C@@H]1CNC[C@H](C)N1
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCN1C[C@@H](C)N[C@@H](C)C1
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
61ec49e5207aa33ebff7094bb66b1d997d4af14524931a8b3643ef7a94219a9a
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCCN1CCNCC1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[#7:4]-[C:9]-[C:8]-1
98
[{"value": 98.0, "product": "ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCN2C[C@H](N[C@H](C2)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
Bromide (207) (60 mg, 0.12 mmol), prepared as described in example 176, was reacted with cis-2,6-dimethylpiperazine according to the procedure described in example 179 except that the reaction was performed at room temperature for 20 h, to give amine (218) (63 mg, 98%) as a yellow powder, mp 199–202° C. 1H NMR δ [(CD3)...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CNCCN1
C1C[NH]CCN1
c1ccccc1.C1C[NH]CCN1.C1NCc2c1ccc1nc3ccccc3c21
HBr
null
null
20
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCBr.C[C@@H]1CNC[C@H](C)N1>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCCN1C[C@@H](C)N[C@@H](C)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6296394591cb4d9196dd59a65c6dc03f
CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O.Sc1ccccc1>>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCSc1ccccc1
CS(=O)(=O)OCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(NC3=O)=O)O.C1(=CC=CC=C1)S.C(C)N(CC)CC>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCSC2=CC=CC=C2
CS(=O)(=O)O[CH2:28][CH2:27][n:26]1[c:17]2[cH:16][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:7]3[c:6]([c:18]2[c:19]2[cH:20][c:21]([OH:22])[cH:23][cH:24][c:25]21)[C:4](=[O:5])[NH:3][C:2]3=[O:1].[SH:29][c:30]1[cH:31][cH:32][cH:33][cH:34][cH:35]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:1...
CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O.Sc1ccccc1
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCSc1ccccc1
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
bb86271f960c642587dc900180f99bfb3d3eab3ca39b11b3cb70560d94f407f0
16472cd174cc2da3287c614705959a9f9d18ac963bc8ef0c26feb5dd489d747b
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCSc1ccccc1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[#7;a:3].[SH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[#7;a:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
27
[{"value": 27.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCSC2=CC=CC=C2", "details": "PERCENTYIELD", "is_desired": false}]
110
CELSIUS
null
null
Mesylate (229) (55 mg, 0.11 mmol) prepared as decribed in example 171 was reacted with excess thiophenol (0.10 mL) according to the procedure described in example 179, except that triethylamine (2.0 mL) was added and the reaction was heated at 110° C. for 4 days. Addition of water was followed by extracted of the compo...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Aromatic thiol
Monosulfide
null
null
c1ccccc1.c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
MsOH.HO-
O
110
null
CS(=O)(=O)OCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O.Sc1ccccc1>O>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCSc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b89c3cc6000840ceb21cafb05db13925
Nc1ccccc1C(=O)O.O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr>>O=C(O)c1ccccc1NCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(NC3=O)=O)O.C1=CC=C(C(=C1)C(=O)O)N>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCNC2=C(C(=O)O)C=CC=C2
[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[NH2:10].Br[CH2:11][CH2:12][CH2:13][n:14]1[c:15]2[cH:16][cH:17][c:18]([OH:19])[cH:20][c:21]2[c:22]2[c:23]3[c:24]([c:25](-[c:26]4[cH:27][cH:28][cH:29][cH:30][c:31]4[Cl:32])[cH:33][c:34]12)[C:35](=[O:36])[NH:37][C:38]3=[O:39]>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][cH...
Nc1ccccc1C(=O)O.O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr
O=C(O)c1ccccc1NCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
fc19a1445ff204e66e51735d0191465bda3c6691fd233624a54742c9d4828411
0b1d32f56ad00f1e5bdae9390f9227bbea012fa2f8203aac34726b8a6761cc7c
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCCNc1ccccc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[c:7]-[C:8](=[O;D1;H0:9])-[O;D1;H1:10]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[NH;D2;+0:4]-[c:5](:[c:6]):[c:7]-[C:8](=[O;D1;H0:9])-[O;D1;H1:10]
88
[{"value": 88.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCNC2=C(C(=O)O)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of the bromide (58) prepared as described in example 172 with o-anthranilic acid using the procedure described in example 179 gave the aniline (60) (88%), mp 261–263° C. 1H NMR δ [(CD3)2SO] 11.05 (s, 1H), 9.38 (s, 1H), 8.39 (d, J=2.4 Hz, 1H), 7.76 (m, 1H), 7.75 (s, 1H), 7.59 (d, J=8.7 Hz, 1H), 7.55 (m, 1H), 7....
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary amine
Secondary amine
null
null
c1ccccc1.c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
HBr
null
null
null
Nc1ccccc1C(=O)O.O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr>>O=C(O)c1ccccc1NCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-abff0e57043e4cab848989dfd590d22d
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr>>CSCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(NC3=O)=O)O.[Li].[Li]SC>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCSC
Br[CH2:3][CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[c:15]3[c:16]([c:17](-[c:18]4[cH:19][cH:20][cH:21][cH:22][c:23]4[Cl:24])[cH:25][c:26]12)[C:27](=[O:28])[NH:29][C:30]3=[O:31]>>[CH3:1][S:2][CH2:3][CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[c:15]3[c:16]([c:1...
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr
CSCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
null
null
O.O1CCOCC1
Miscellaneous
OtherReaction
c7f6703d8c9a47e72372c222cbd53ce8b0f05c02a135956dea2f6ecbca239ce6
acbc727a20407483543a5245cd99740ae3639831d576fa39047899f0e1fe81f3
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Br-[CH2;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[#16:4]-[C;D1;H3:5]
null
[]
null
null
9
HOUR
A mixture of the bromide (58) (60.0 mg, 0.124 mmol) prepared as described in example 172 and lithium thiomercaptide (13 mg, 0.2481 mmol) in p-dioxane (5 mL) was refluxed for 16 h. A further 10 mg of LiSMe was added and refluxing was continued for a further 9 h. The mixture was diluted with water, extracted with ethyl a...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Monosulfide
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Br-
O.O1CCOCC1
null
9
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr>O.O1CCOCC1>CSCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d5151d0c90e84864901a4cd4c077061f
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr.Sc1ccccc1>>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCSc1ccccc1
O.BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(NC3=O)=O)O.C1(=CC=CC=C1)S.C(C)N(CC)CC>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCCSC2=CC=CC=C2
Br[CH2:29][CH2:28][CH2:27][n:26]1[c:17]2[cH:16][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:7]3[c:6]([c:18]2[c:19]2[cH:20][c:21]([OH:22])[cH:23][cH:24][c:25]21)[C:4](=[O:5])[NH:3][C:2]3=[O:1].[SH:30][c:31]1[cH:32][cH:33][cH:34][cH:35][cH:36]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10...
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr.Sc1ccccc1
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCSc1ccccc1
null
null
O1CCOCC1
Heteroatom Alkylation and Arylation
thioether_nucl_sub
26df88c6a3f5f203c89584658be4e126cb42994c98a2e16bc812e1036cdae857
8b2f52296c3a93039174c980b6042ba15754e04d6892a1284c3a32985220b214
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCCSc1ccccc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[SH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
null
[]
null
null
null
null
A solution of the bromide (58) (41 mg, 0.085 mmol) prepared as described in example 172, thiophenol (9.5 μL, 0.093 mmol) and triethylamine (0.25 mL, 3.40 mmol) in p-dioxane (1.5 mL) was refluxed for 16 h. Water was added and the mixture was extracted with ethyl acetate. The organic layer was dried, the drying agent was...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic thiol
Monosulfide
null
null
c1ccccc1.c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
HBr
O1CCOCC1
null
null
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr.Sc1ccccc1>O1CCOCC1>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCSc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2074e4d1b268405a81592841c2097642
CO.C[O-].O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr>>COCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)OC3=O
Cl.BrCCCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(NC3=O)=O)O.CO.C[O-].[Na+]>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(OC2=O)=O)O)CCCOC
C[OH:29].[CH3:1][O-:2].Br[CH2:3][CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[c:15]3[c:16]([c:17](-[c:18]4[cH:19][cH:20][cH:21][cH:22][c:23]4[Cl:24])[cH:25][c:26]12)[C:27](=[O:28])N[C:30]3=[O:31]>>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[...
CO.C[O-].O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr
COCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)OC3=O
null
null
O1CCOCC1
Acylation
OtherReaction
aa74ae21e92556b7bfc022aa15b13c3d72fc3a4f78b3baac80a97b35a10dc16e
28d1aeeff3505343953582dd13040e5ccf99afb73b2ea1712b3b26d6f4b25824
O=C1OC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Br-[CH2;D2;+0:1]-[C:2]-[C:3]-[#7;a:4]:[c:5]:[c:6]:[c:7]1:[c:8](:[c:9])-[C;H0;D3;+0:10](=[O;D1;H0:11])-N-[C;H0;D3;+0:12]-1=[O;D1;H0:13].C-[OH;D1;+0:14].[C;D1;H3:15]-[O-;H0;D1:16]>>[C;D1;H3:15]-[O;H0;D2;+0:16]-[CH2;D2;+0:1]-[C:2]-[C:3]-[#7;a:4]:[c:5]:[c:6]:[c:7]1:[c:8](:[c:9])-[C;H0;D3;+0:10](=[O;D1;H0:11])-[O;H0;D2;+0:1...
null
[]
null
null
null
null
A solution of the bromide (58) (50 mg, 0.103 mmol) prepared as described in example 172 and sodium methoxide (35.2 mg, 0.65 mmol) in methanol (0.5 mL) and p-dioxane (8 mL) was refluxed for 3 h. The solution was acidified with 2N HCl, extracted with ethyl acetate and the organic layer was dried, the drying agent was rem...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Unsubstituted dicarboximide.Methanol
Anhydride.Ester.Ester.Ether
C1NCc2c1ccc1[nH]c3ccccc3c21
C1OCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.C1OCc2c1ccc1[nH]c3ccccc3c21
HBr
O1CCOCC1
null
null
CO.C[O-].O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCCBr>O1CCOCC1>COCCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)OC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b197a92233c64fc5a8d67b98bc499b20
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(=O)O)C(=O)NC3=O.N>>COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O
ClC1=C(C(=CC=C1)Cl)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)O.N>>ClC1=C(C(=CC=C1)Cl)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)N
O[C:26]([CH2:25][CH2:24][n:23]1[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8][c:7]2[c:9]2[c:10]3[c:11]([c:12](-[c:13]4[c:14]([Cl:15])[cH:16][cH:17][cH:18][c:19]4[Cl:20])[cH:21][c:22]21)[C:29](=[O:30])[NH:31][C:32]3=[O:33])=[O:28].[NH3:27]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[c:9]1[c:10]3[c:11]([c:12](-[c:13...
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(=O)O)C(=O)NC3=O.N
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O
null
null
null
Acylation
Carboxylic acid to amide conversion
1283aef55d7ee699f097a8e5267689198c76ba671644401547f902657820236d
cb0a71c3fb37a76e96fbd81aae6f95a28398a03d1ad2c8e877085e735efb98f1
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[NH3;D0;+0:5]>>[C:4]-[C:3]-[C;H0;D3;+0:1](-[NH2;D1;+0:5])=[O;D1;H0:2]
73
[{"value": 73.0, "product": "ClC1=C(C(=CC=C1)Cl)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)N", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of acid (244) (0.23 g, 0.48 mmol) prepared as described in example 204 according to the procedure described in example 207, except that concentrated ammonia (˜30%, 20 mL) was added as the amine, gave amide (250) (0.17 g, 73%) as a yellow powder, mp 261–264° C. 1H NMR δ [(CD3)2SO] 11.19 (br s, 1H), 8.50 (d, J=2...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary amide
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
HO-
null
null
null
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(=O)O)C(=O)NC3=O.N>>COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-63b33118c5334130939d6c3e5f27f1ba
COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCC(=O)NCCN(C)C)C(=O)NC3=O>>CN(C)CCNC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
CN(CCNC(CCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)OC)=O)C.N>>CN(CCNC(CCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O)=O)C
C[O:16][c:15]1[cH:14][cH:13][c:12]2[n:11]([CH2:10][CH2:9][C:7]([NH:6][CH2:5][CH2:4][N:2]([CH3:1])[CH3:3])=[O:8])[c:30]3[c:19]([c:18]2[cH:17]1)[c:20]1[c:21]([c:22](-[c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[cH:29]3)[C:31](=[O:32])[NH:33][C:34]1=[O:35]>>[CH3:1][N:2]([CH3:3])[CH2:4][CH2:5][NH:6][C:7](=[O:8])[CH2:9][CH2...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCC(=O)NCCN(C)C)C(=O)NC3=O
CN(C)CCNC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
null
null
O
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
Reaction of methyl ether (247) (70 mg, 0.14 mmol) prepared as described in example 207 according to the procedure described in example 81, except that the reaction mixture was diluted with water, basified by the addition of concentrated ammonia and extracted with ethyl acetate. The organic layer was dried, the drying a...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
O
null
null
COc1ccc2c(c1)c1c3c(c(-c4ccccc4)cc1n2CCC(=O)NCCN(C)C)C(=O)NC3=O>O>CN(C)CCNC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-43b0467513d5487d801b433d3756f736
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O>>NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4c(Cl)cccc4Cl)cc21)C(=O)NC3=O
ClC1=C(C(=CC=C1)Cl)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)N.O1CCCC1>>ClC1=C(C(=CC=C1)Cl)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)N
C[O:11][c:10]1[cH:9][cH:8][c:7]2[n:6]([CH2:5][CH2:4][C:2]([NH2:1])=[O:3])[c:27]3[c:14]([c:13]2[cH:12]1)[c:15]1[c:16]([c:17](-[c:18]2[c:19]([Cl:20])[cH:21][cH:22][cH:23][c:24]2[Cl:25])[cH:26]3)[C:28](=[O:29])[NH:30][C:31]1=[O:32]>>[NH2:1][C:2](=[O:3])[CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:...
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O
NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4c(Cl)cccc4Cl)cc21)C(=O)NC3=O
null
null
C(C)(=O)OCC
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
59
[{"value": 59.0, "product": "ClC1=C(C(=CC=C1)Cl)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 59.0, "product": "ClC1=C(C(=CC=C1)Cl)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of methyl ether (250) (80 mg, 0.17 mmol)) prepared as described in example 210 according to The procedure described in example 80, followed by chromatography on silica eluting with ethyl acetate then tetrahydrofuran and trituration from ethyl acetate, gave amide (258) (47 mg, 59%) as an orange powder, mp 327–3...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
C(C)(=O)OCC
null
null
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O>C(C)(=O)OCC>NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4c(Cl)cccc4Cl)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-66d5617ee3174b04900152f40608af0f
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCC(=O)NCCN(C)C)C(=O)NC3=O.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCn1ccnc1>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C
ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NCCN(C)C.OC1=CC=2C=3C4=C(C(=CC3N(C2C=C1)CCCN1C=NC=C1)C1=CC=CC=C1)C(NC4=O)=O>>ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NCCN(C)C
COc1ccc2c(c1)[c:13]1[c:12]([cH:11][c:10](-[c:9]3[c:3]([O:2][CH3:1])[cH:4][cH:5][cH:6][c:7]3[Cl:8])[c:15]3[c:14]1[C:19](=[O:20])[NH:18][C:16]3=[O:17])[n:28]2[CH2:29][CH2:30][C:31](=[O:32])[NH:33][CH2:34][CH2:35][N:36]([CH3:37])[CH3:38].O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2[c:21]2[cH:22][c:23]([OH:24])[cH:25][cH:26][c:27]2n1CC...
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCC(=O)NCCN(C)C)C(=O)NC3=O.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCn1ccnc1
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C
null
null
null
Miscellaneous
OtherReaction
04e2bfa40d4eefbd80f022dff1597ce73473c2e77c3cc98a6101158bfaeb33ee
0404f73f8bae062b3c383035c98e95881c2a09658febdbde66fa05b90ea55863
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-O-c1:c:c:c2:[n;H0;D3;+0:1](-[C:2]-[C:3]-[C:4](-[#7:5])=[O;D1;H0:6]):[c:7](:[c:8]):[c;H0;D3;+0:9](:[c:10]3:[c:11]-[C:12](=[O;D1;H0:13])-[#7:14]-[C:15]-3=[O;D1;H0:16]):c:2:c:1.O=C1-N-C(=O)-c2:c-1:c(-c1:c:c:c:c:c:1):c:c1:c:2:[c;H0;D3;+0:17]2:[c:18]:[c:19]:[c:20]:[c:21]:[c;H0;D3;+0:22]:2:n:1-C-C-C-n1:c:c:n:c:1>>[#7:5]-[C...
83
[{"value": 83.0, "product": "ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NCCN(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
Reaction of methyl ether (252) prepared as described in example 212 (80 mg, 0.15 mmol) according to The procedure described in example 80, except that the reaction was performed at 0° C. for 2 hours and chromatography was performed eluting with ethyl acetate/methanol/triethylamine (1:0:0 to 3:1:trace), gave amide (260)...
10.6084/m9.figshare.5104873.v1
null
Ether.Unsubstituted dicarboximide
null
C1NCc2c1ccc1nc3ccccc3c21.c1ccccc1.c1c[nH]cn1.c1ccc2nc3ccc4c(c3c2c1)CNC4
C1NCc2c1ccc1nc3ccccc3c21
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
HO-
null
null
2
COc1ccc2c(c1)c1c3c(c(-c4c(Cl)cccc4OC)cc1n2CCC(=O)NCCN(C)C)C(=O)NC3=O.O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CCCn1ccnc1>>COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2d72889ef0374e16a7cf146871cfef15
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C>>COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C
ClC1=C(C(=CC=C1)OC)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NCCN(C)C>>CN(CCNC(CCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)O)=O)C
Cl[c:7]1[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[c:8]1-[c:9]1[cH:10][c:11]2[c:12]([c:13]3[c:14]1[C:15](=[O:16])[NH:17][C:18]3=[O:19])[c:20]1[cH:21][c:22]([OH:23])[cH:24][cH:25][c:26]1[n:27]2[CH2:28][CH2:29][C:30](=[O:31])[NH:32][CH2:33][CH2:34][N:35]([CH3:36])[CH3:37]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1-[c:9...
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C
COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C
null
[Pd].[Pd]
C(C)(=O)OCC.CO
Functional Group Interconversion
Aromatic dehalogenation
b66818d3926a4463fb8e1c3d4a89e94e47b4d46960d4bdb7bcfbeeec427cfd4e
56de34d4a44cb25d9380269ee5e138b0f24b40a3a0db22c5508049dc775a861f
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[c:5]):[c:6]>>[c:6]:[c:4](-[c:5]):[cH;D2;+0:1]:[c:2]:[c:3]
17.1
[{"value": 16.0, "product": "CN(CCNC(CCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)O)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 17.1, "product": "CN(CCNC(CCN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)OC)C(NC3=O)=O)O)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of amide (260) (40 mg, 0.07 mmol)) prepared as described in example 219 in ethyl acetate/methanol (1:1, 80 mL) was added 5% Pd-C (catalytic). The resulting suspension was hydrogenated at 60 psi with stirring for 4 days, with additional portions of Pd-C being added every 24 hours. The reaction mixture was ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccccc1
c1ccccc1
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
Other
[Pd].[Pd].C(C)(=O)OCC.CO
null
null
COc1cccc(Cl)c1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C>[Pd].[Pd].C(C)(=O)OCC.CO>COc1ccccc1-c1cc2c(c3c1C(=O)NC3=O)c1cc(O)ccc1n2CCC(=O)NCCN(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-786dafbcfc7b4dec85251560283dc0a9
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NS(=O)(=O)CCN(C)C)C(=O)NC3=O>>CN(C)CCS(=O)(=O)NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NS(=O)(=O)CCN(C)C>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NS(=O)(=O)CCN(C)C
C[O:19][c:18]1[cH:17][cH:16][c:15]2[n:14]([CH2:13][CH2:12][C:10]([NH:9][S:6]([CH2:5][CH2:4][N:2]([CH3:1])[CH3:3])(=[O:7])=[O:8])=[O:11])[c:34]3[c:22]([c:21]2[cH:20]1)[c:23]1[c:24]([c:25](-[c:26]2[cH:27][cH:28][cH:29][cH:30][c:31]2[Cl:32])[cH:33]3)[C:35](=[O:36])[NH:37][C:38]1=[O:39]>>[CH3:1][N:2]([CH3:3])[CH2:4][CH2:5]...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NS(=O)(=O)CCN(C)C)C(=O)NC3=O
CN(C)CCS(=O)(=O)NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
null
null
C([O-])(O)=O.[Na+]
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
23.4
[{"value": 23.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NS(=O)(=O)CCN(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 23.4, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NS(=O)(=O)CCN(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired...
null
null
null
null
Reaction of methyl ether (267) (35 mg, 0.06 mmol) prepared as described in example 224 according to the proceedure described in example 81, except that the reaction mixture was diluted with saturated sodium bicarbonate and extracted with ethyl acetate. The organic phase was dried, the drying agent was removed and the s...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
C([O-])(O)=O.[Na+]
null
null
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NS(=O)(=O)CCN(C)C)C(=O)NC3=O>C([O-])(O)=O.[Na+]>CN(C)CCS(=O)(=O)NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6204db7a9e304c63b085f7c35e35f930
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)O)C(=O)NC3=O>>O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)O.Cl.[NH+]1=CC=CC=C1>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)O
C[O:11][c:10]1[cH:9][cH:8][c:7]2[n:6]([CH2:5][CH2:4][C:2](=[O:1])[OH:3])[c:26]3[c:14]([c:13]2[cH:12]1)[c:15]1[c:16]([c:17](-[c:18]2[cH:19][cH:20][cH:21][cH:22][c:23]2[Cl:24])[cH:25]3)[C:27](=[O:28])[NH:29][C:30]1=[O:31]>>[O:1]=[C:2]([OH:3])[CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[c:15]...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)O)C(=O)NC3=O
O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
50
[{"value": 50.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Demethylation of (116) prepared as described in example 229 with pyridinium hydrochloride using the procedure described in example 81 gave (117) (50%) as a yellow powder, mp 286° C. 1H NMR δ [(CD3)2SO] 12.40 (br, 1H), 11.06 (br s, 1H), 9.37 (br s, 1H), 8.37 (d, J=2.4 Hz, 1H), 7.81 (s, 1H), 7.59 (d, J=8.7 Hz, 1H), 7.57 ...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
null
null
null
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)O)C(=O)NC3=O>>O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0f624640443e434cbe5f5c9f361c5e94
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O>>NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)N.B(Br)(Br)Br>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)N
C[O:11][c:10]1[cH:9][cH:8][c:7]2[n:6]([CH2:5][CH2:4][C:2]([NH2:1])=[O:3])[c:26]3[c:14]([c:13]2[cH:12]1)[c:15]1[c:16]([c:17](-[c:18]2[cH:19][cH:20][cH:21][cH:22][c:23]2[Cl:24])[cH:25]3)[C:27](=[O:28])[NH:29][C:30]1=[O:31]>>[NH2:1][C:2](=[O:3])[CH2:4][CH2:5][n:6]1[c:7]2[cH:8][cH:9][c:10]([OH:11])[cH:12][c:13]2[c:14]2[c:1...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O
NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
77
[{"value": 77.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)N", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Demethylation of (118) prepared as described in example 231 with BBr3 using the procedure described in example 80 gave (119) as a yellow/orange powder (77%), mp 319–322° C. 1H NMR δ [(CD3)2SO] 11.06 (br s, 1H), 9.36 (br s, 1H), 8.37 (d, J=2.4 Hz, 1H), 7.77 (s, 1H), 7.60–7.55 (m, 2H), 7.52–7.43 (m, 3H), 7.35 (br, 1H), 7...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
null
null
null
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(N)=O)C(=O)NC3=O>>NC(=O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ebf2c83b161a4451bd0502da9dbb9704
NCCN1CCOCC1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCN1CCOCC1)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)O.C(C(=O)Cl)(=O)Cl.NCCN1CCOCC1>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NCCN2CCOCC2
[NH2:27][CH2:28][CH2:29][N:30]1[CH2:31][CH2:32][O:33][CH2:34][CH2:35]1.O[C:25]([CH2:24][CH2:23][n:22]1[c:6]2[cH:5][cH:4][c:3]([OH:2])[cH:8][c:7]2[c:9]2[c:10]3[c:11]([c:12](-[c:13]4[cH:14][cH:15][cH:16][cH:17][c:18]4[Cl:19])[cH:20][c:21]21)[C:36](=[O:37])[NH:38][C:39]3=[O:40])=[O:26]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]...
NCCN1CCOCC1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCN1CCOCC1)C(=O)NC3=O
null
null
null
Acylation
OtherReaction
e490eebb477043dc0542732dd7a6ce49276641802836b4489c620def21f9d46c
fcf68d457905b35c628fee285772653b3fd6812b4e55ecf3f563dfc9713d647a
O=C(CCn1c2ccccc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O)NCCN1CCOCC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8].[C:9]-[C:10]-[NH2;D1;+0:11]>>[C;D1;H3:12]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8].[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:11]-[C:10]-[C:9]
73
[{"value": 73.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NCCN2CCOCC2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of acid (117) prepared as described in example 230 with oxalyl chloride followed by N-(2-aminoethyl)morpholine using the procedure described in example 207 gave the amide (120) (73%) as a yellow powder, mp 174–176° C. 1H NMR δ [(CD3)2SO] 11.12 (br s, 1H), 8.51 (d, J=2.6 Hz, 1H), 7.77 (s, 1H), 7.74 (t, J=5.6 Hz...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Aromatic alcohol.Primary amine
Ether.Secondary amide
null
null
c1ccccc1.C1COCC[NH]1.C1NCc2c1ccc1[nH]c3ccccc3c21
null
null
null
null
NCCN1CCOCC1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCN1CCOCC1)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7b6a5fef751a4360973346568a5ff73a
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCN1CCOCC1)C(=O)NC3=O>>O=C(CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O)NCCN1CCOCC1
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NCCN2CCOCC2.B(Br)(Br)Br>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NCCN2CCOCC2
C[O:10][c:9]1[cH:8][cH:7][c:6]2[n:5]([CH2:4][CH2:3][C:2](=[O:1])[NH:31][CH2:32][CH2:33][N:34]3[CH2:35][CH2:36][O:37][CH2:38][CH2:39]3)[c:25]3[c:13]([c:12]2[cH:11]1)[c:14]1[c:15]([c:16](-[c:17]2[cH:18][cH:19][cH:20][cH:21][c:22]2[Cl:23])[cH:24]3)[C:26](=[O:27])[NH:28][C:29]1=[O:30]>>[O:1]=[C:2]([CH2:3][CH2:4][n:5]1[c:6]...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCN1CCOCC1)C(=O)NC3=O
O=C(CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O)NCCN1CCOCC1
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C(CCn1c2ccccc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O)NCCN1CCOCC1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
64
[{"value": 64.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NCCN2CCOCC2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
Demethylation of (120) prepared as described in example 233 with BBr3 using the procedure described in example 80 except that the reaction time was 16 h gave (121) as a yellow powder (64%), mp 143–148° C. (dec). 1H NMR δ [(CD3)2SO] 11.05 (s, 1H), 9.35 (s, 1H), 8.36 (d, J=2.4 Hz, 1H), 7.74 (t, J=5.6 Hz, 1H), 7.71 (s, 1H...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.C1COCC[NH]1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
null
null
16
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCN1CCOCC1)C(=O)NC3=O>>O=C(CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O)NCCN1CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-87762ef3bc394568a794bebe60f282eb
CC1(C)CC(N)CC(C)(C)N1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NC1CC(C)(C)NC(C)(C)C1)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)O.C(C(=O)Cl)(=O)Cl.NC1CC(NC(C1)(C)C)(C)C>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NC2CC(NC(C2)(C)C)(C)C
[NH2:27][CH:28]1[CH2:29][C:30]([CH3:31])([CH3:32])[NH:33][C:34]([CH3:35])([CH3:36])[CH2:37]1.O[C:25]([CH2:24][CH2:23][n:22]1[c:6]2[cH:5][cH:4][c:3]([OH:2])[cH:8][c:7]2[c:9]2[c:10]3[c:11]([c:12](-[c:13]4[cH:14][cH:15][cH:16][cH:17][c:18]4[Cl:19])[cH:20][c:21]21)[C:38](=[O:39])[NH:40][C:41]3=[O:42])=[O:26]>>[CH3:1][O:2][...
CC1(C)CC(N)CC(C)(C)N1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NC1CC(C)(C)NC(C)(C)C1)C(=O)NC3=O
null
null
null
Acylation
OtherReaction
e490eebb477043dc0542732dd7a6ce49276641802836b4489c620def21f9d46c
fcf68d457905b35c628fee285772653b3fd6812b4e55ecf3f563dfc9713d647a
O=C(CCn1c2ccccc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O)NC1CCNCC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8].[C:9]-[C:10](-[NH2;D1;+0:11])-[C:12]>>[C;D1;H3:13]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8].[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:11]-[C:10](-[C:9])-[C:12]
72
[{"value": 72.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NC2CC(NC(C2)(C)C)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of acid (117) prepared as described in example 230 with oxalyl chloride followed by 4-amino-(2,2,6,6-tetramethyl)piperidine using the procedure described in example 207 gave the amide (124) (72%) as a yellow powder, mp 155–160° C. (dec). 1H NMR δ [(CD3)2SO] 11.12 (br, 1H), 8.51 (d, J=2.6 Hz, 1H), 7.78 (s, 1H),...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Aromatic alcohol.Primary amine
Ether.Secondary amide
null
null
c1ccccc1.C1CCNCC1.C1NCc2c1ccc1[nH]c3ccccc3c21
null
null
null
null
CC1(C)CC(N)CC(C)(C)N1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NC1CC(C)(C)NC(C)(C)C1)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-23f0286140094cc399e0b44e036c79d9
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NC1CC(C)(C)NC(C)(C)C1)C(=O)NC3=O>>CC1(C)CC(NC(=O)CCn2c3ccc(O)cc3c3c4c(c(-c5ccccc5Cl)cc32)C(=O)NC4=O)CC(C)(C)N1
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NC2CC(NC(C2)(C)C)(C)C.B(Br)(Br)Br>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NC2CC(NC(C2)(C)C)(C)C
C[O:16][c:15]1[cH:14][cH:13][c:12]2[n:11]([CH2:10][CH2:9][C:7]([NH:6][CH:5]3[CH2:4][C:2]([CH3:1])([CH3:3])[NH:41][C:38]([CH3:39])([CH3:40])[CH2:37]3)=[O:8])[c:31]3[c:19]([c:18]2[cH:17]1)[c:20]1[c:21]([c:22](-[c:23]2[cH:24][cH:25][cH:26][cH:27][c:28]2[Cl:29])[cH:30]3)[C:32](=[O:33])[NH:34][C:35]1=[O:36]>>[CH3:1][C:2]1([...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NC1CC(C)(C)NC(C)(C)C1)C(=O)NC3=O
CC1(C)CC(NC(=O)CCn2c3ccc(O)cc3c3c4c(c(-c5ccccc5Cl)cc32)C(=O)NC4=O)CC(C)(C)N1
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C(CCn1c2ccccc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O)NC1CCNCC1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
47
[{"value": 47.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NC2CC(NC(C2)(C)C)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
48
HOUR
Demethylation of (124) prepared as described in example 237 with BBr3 using the procedure described in example 80 except that the reaction time was 48 h gave (125) as a yellow powder (47%), mp 293–299° C. (dec). 1H NMR δ [(CD3)2SO] 11.08 (br s, 1H), 9.38 (br s, 1H), 8.72 (br, 1H), 8.37 (d, J=2.4 Hz, 1H), 7.83 (d, J=7.1...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
C1CCNCC1.c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
null
null
48
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NC1CC(C)(C)NC(C)(C)C1)C(=O)NC3=O>>CC1(C)CC(NC(=O)CCn2c3ccc(O)cc3c3c4c(c(-c5ccccc5Cl)cc32)C(=O)NC4=O)CC(C)(C)N1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bf82ca84eb494da698eff1c7d6330ab7
C[C@@H]1CNC[C@H](C)N1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)N1C[C@@H](C)N[C@@H](C)C1)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)O.C(C(=O)Cl)(=O)Cl.C[C@@H]1N[C@@H](CNC1)C>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)N2C[C@H](N[C@H](C2)C)C
[NH:27]1[CH2:28][C@@H:29]([CH3:30])[NH:31][C@@H:32]([CH3:33])[CH2:34]1.O[C:25]([CH2:24][CH2:23][n:22]1[c:6]2[cH:5][cH:4][c:3]([OH:2])[cH:8][c:7]2[c:9]2[c:10]3[c:11]([c:12](-[c:13]4[cH:14][cH:15][cH:16][cH:17][c:18]4[Cl:19])[cH:20][c:21]21)[C:35](=[O:36])[NH:37][C:38]3=[O:39])=[O:26]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]...
C[C@@H]1CNC[C@H](C)N1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)N1C[C@@H](C)N[C@@H](C)C1)C(=O)NC3=O
null
null
null
Acylation
OtherReaction
d5514a6760e82f876a7c9f84c493e9b26fbd78acff107645e987694b09882cec
71f673d14b505054b867264e6efffeeae2c2502635894b4948f22bc3c49a295b
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCC(=O)N1CCNCC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8].[#7:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[C;D1;H3:15]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8].[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:12]1-[C:11]-[C:10]-[#7:9]-[C:14]-[C:13]-1
76
[{"value": 76.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)N2C[C@H](N[C@H](C2)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of acid (117) prepared as described in example 230 with oxalyl chloride followed by cis-2,6-dimethylpiperazine using the procedure described in example 207 gave the amide (126) (76%) as a yellow powder, mp 168–173° C. (dec). 1H NMR δ [(CD3)2SO] 11.13 (br, 1H), 8.52 (d, J=2.6 Hz, 1H), 7.80 (s, 0.5H), 7.76 (s, 0...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Aromatic alcohol.Secondary amine
Ether.Tertiary amide
C1CNCCN1
C1C[NH]CCN1
c1ccccc1.C1C[NH]CCN1.C1NCc2c1ccc1[nH]c3ccccc3c21
null
null
null
null
C[C@@H]1CNC[C@H](C)N1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)N1C[C@@H](C)N[C@@H](C)C1)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fc10689e4ed84f96812f897b3db7adea
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)N1C[C@@H](C)N[C@@H](C)C1)C(=O)NC3=O>>C[C@@H]1CN(C(=O)CCn2c3ccc(O)cc3c3c4c(c(-c5ccccc5Cl)cc32)C(=O)NC4=O)C[C@H](C)N1
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)N2C[C@H](N[C@H](C2)C)C.B(Br)(Br)Br>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)N2C[C@H](N[C@H](C2)C)C
C[O:14][c:13]1[cH:12][cH:11][c:10]2[n:9]([CH2:8][CH2:7][C:5]([N:4]3[CH2:3][C@@H:2]([CH3:1])[NH:38][C@@H:36]([CH3:37])[CH2:35]3)=[O:6])[c:29]3[c:17]([c:16]2[cH:15]1)[c:18]1[c:19]([c:20](-[c:21]2[cH:22][cH:23][cH:24][cH:25][c:26]2[Cl:27])[cH:28]3)[C:30](=[O:31])[NH:32][C:33]1=[O:34]>>[CH3:1][C@@H:2]1[CH2:3][N:4]([C:5](=[...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)N1C[C@@H](C)N[C@@H](C)C1)C(=O)NC3=O
C[C@@H]1CN(C(=O)CCn2c3ccc(O)cc3c3c4c(c(-c5ccccc5Cl)cc32)C(=O)NC4=O)C[C@H](C)N1
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCC(=O)N1CCNCC1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
38
[{"value": 38.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)N2C[C@H](N[C@H](C2)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
48
HOUR
Demethylation of (126) prepared as described in example 239 (with BBr3 using the procedure described in example 80 except that the reaction time was 48 h gave (127) as a yellow powder (38%), mp 220–224° C. (dec). 1H NMR δ [(CD3)2SO] 11.07 (br s, 1H) 9.36 (br s, 1H), 8.72 (br, 1H), 8.34 br, 1H), 7.72 (s, 0.5H), 7.71 (s,...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
C1CNCC[NH]1.c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
null
null
48
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)N1C[C@@H](C)N[C@@H](C)C1)C(=O)NC3=O>>C[C@@H]1CN(C(=O)CCn2c3ccc(O)cc3c3c4c(c(-c5ccccc5Cl)cc32)C(=O)NC4=O)C[C@H](C)N1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-433c46922dbe4aab9fda6d1573802cf3
NCCc1c[nH]cn1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCc1cnc[nH]1)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)O.C(C(=O)Cl)(=O)Cl.NCCC1=CNC=N1>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NCCC2=CN=CN2
[NH2:27][CH2:28][CH2:29][c:30]1[cH:31][nH:32][cH:33][n:34]1.O[C:25]([CH2:24][CH2:23][n:22]1[c:6]2[cH:5][cH:4][c:3]([OH:2])[cH:8][c:7]2[c:9]2[c:10]3[c:11]([c:12](-[c:13]4[cH:14][cH:15][cH:16][cH:17][c:18]4[Cl:19])[cH:20][c:21]21)[C:35](=[O:36])[NH:37][C:38]3=[O:39])=[O:26]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:...
NCCc1c[nH]cn1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCc1cnc[nH]1)C(=O)NC3=O
null
null
null
Acylation
OtherReaction
e490eebb477043dc0542732dd7a6ce49276641802836b4489c620def21f9d46c
fcf68d457905b35c628fee285772653b3fd6812b4e55ecf3f563dfc9713d647a
O=C(CCn1c2ccccc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O)NCCc1cnc[nH]1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8].[NH2;D1;+0:9]-[C:10]-[C:11]-[c:12]1:[c:13]:[nH;D2;+0:14]:[c:15]:[n;H0;D2;+0:16]:1>>[C;D1;H3:17]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8].[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:9]-[C:10]-[C:11]-[c:12]1:[c:13]:[n;H0;D2;+0:14]:[c:15]:[nH;D2;...
81
[{"value": 81.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NCCC2=CN=CN2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of acid (117) prepared as described in example 230 with oxalyl chloride followed by histamine using the procedure described in example 207 gave the amide (128) (81%) as a yellow powder, mp 144–149° C. (dec). 1H NMR δ [(CD3)2SO] 11.12 (br, 1H), 8.52 (d, J=2.6 Hz, 1H), 7.91 (t, J=5.5 Hz, 1H), 7.76 (s, 1H), 7.69 ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Aromatic alcohol.Primary amine
Ether.Secondary amide
null
null
c1ccccc1.c1c[nH]cn1.C1NCc2c1ccc1[nH]c3ccccc3c21
null
null
null
null
NCCc1c[nH]cn1.O=C(O)CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O>>COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCc1cnc[nH]1)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2b59472ebce341ce8560e7ca3d38bb3e
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCc1cnc[nH]1)C(=O)NC3=O>>O=C(CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O)NCCc1cnc[nH]1
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)OC)CCC(=O)NCCC2=CN=CN2.B(Br)(Br)Br>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NCCC2=CN=CN2
C[O:10][c:9]1[cH:8][cH:7][c:6]2[n:5]([CH2:4][CH2:3][C:2](=[O:1])[NH:31][CH2:32][CH2:33][c:34]3[cH:35][n:36][cH:37][nH:38]3)[c:25]3[c:13]([c:12]2[cH:11]1)[c:14]1[c:15]([c:16](-[c:17]2[cH:18][cH:19][cH:20][cH:21][c:22]2[Cl:23])[cH:24]3)[C:26](=[O:27])[NH:28][C:29]1=[O:30]>>[O:1]=[C:2]([CH2:3][CH2:4][n:5]1[c:6]2[cH:7][cH:...
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCc1cnc[nH]1)C(=O)NC3=O
O=C(CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O)NCCc1cnc[nH]1
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C(CCn1c2ccccc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O)NCCc1cnc[nH]1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
46
[{"value": 46.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC(=O)NCCC2=CN=CN2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
48
HOUR
Demethylation of (128) prepared as described in example 241 with BBr3 using the procedure described in example 80 except that the reaction time was 48 h gave (129) as a yellow powder (46%), mp 158–162° C. (dec). 1H NMR δ [(CD3)2SO] 11.75 (br, 1H), 11.05 (br s, 1H), 9.36 (br s, 1H), 8.37 (d, J=2.4 Hz, 1H), 7.91 (t, J=5....
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.c1c[nH]cn1.C1NCc2c1ccc1[nH]c3ccccc3c21
Other
null
null
48
COc1ccc2c(c1)c1c3c(c(-c4ccccc4Cl)cc1n2CCC(=O)NCCc1cnc[nH]1)C(=O)NC3=O>>O=C(CCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O)NCCc1cnc[nH]1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d9e8ac3d46b14af1810494a565aed42a
COC(=O)CN=[N+]=[N-].COc1cc(C=O)ccc1OCc1ccccc1>>COC(=O)C(=Cc1ccc(OCc2ccccc2)c(OC)c1)N=[N+]=[N-]
C(C1=CC=CC=C1)OC1=C(C=C(C=O)C=C1)OC.N(=[N+]=[N-])CC(=O)OC.[Na].C[O-].[Na+]>>COC(C(=CC1=CC(=C(C=C1)OCC1=CC=CC=C1)OC)N=[N+]=[N-])=O
[CH3:1][O:2][C:3](=[O:4])[CH2:5][N:23]=[N+:24]=[N-:25].O=[CH:6][c:7]1[cH:8][cH:9][c:10]([O:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[c:19]([O:20][CH3:21])[cH:22]1>>[CH3:1][O:2][C:3](=[O:4])[C:5](=[CH:6][c:7]1[cH:8][cH:9][c:10]([O:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[c:19]([O:20][CH3:21]...
COC(=O)CN=[N+]=[N-].COc1cc(C=O)ccc1OCc1ccccc1
COC(=O)C(=Cc1ccc(OCc2ccccc2)c(OC)c1)N=[N+]=[N-]
null
null
CO
C-C Coupling
Aldol condensation
a86984aeb4a9963534e0b081b0ecca18455fda1775f36ce168d1ca4cf966df3e
203dd34a20dceaf1737adbf20e01b43c2424e4e4b1722d942d1a796d895396e6
c1ccc(COc2ccccc2)cc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C;D1;H3:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[CH2;D2;+0:9]-[#7:10]=[#7;+:11]=[N;-;D1;H0:12]>>[C;D1;H3:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[C;H0;D3;+0:9](-[#7:10]=[#7;+:11]=[N;-;D1;H0:12])=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]
73
[{"value": 73.0, "product": "COC(C(=CC1=CC(=C(C=C1)OCC1=CC=CC=C1)OC)N=[N+]=[N-])=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.5, "product": "COC(C(=CC1=CC(=C(C=C1)OCC1=CC=CC=C1)OC)N=[N+]=[N-])=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
45
MINUTE
A solution of the 4-Benzyloxy-3-methoxy-benzaldehyde (12.0 g, 49.6 mmol) and methyl azidoacetate (23 g, 0.200 mol) in methanol (50 mL) was added over 30 min to a cooled (ice-salt bath) solution of sodium methoxide which had been prepared from addition of methanol (80 mL) to sodium (3.4 g, 0.149 mol). The reaction mixtu...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester
Ester
null
null
c1ccccc1.c1ccccc1
HO-
CO
0
0.75
COC(=O)CN=[N+]=[N-].COc1cc(C=O)ccc1OCc1ccccc1>CO>COC(=O)C(=Cc1ccc(OCc2ccccc2)c(OC)c1)N=[N+]=[N-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5b03fb00651042f0af60dea939965173
COC(=O)C(=Cc1ccc(OCc2ccccc2)c(OC)c1)N=[N+]=[N-]>>COC(=O)c1cc2cc(OC)c(OCc3ccccc3)cc2[nH]1
COC(C(=CC1=CC(=C(C=C1)OCC1=CC=CC=C1)OC)N=[N+]=[N-])=O>>COC(=O)C=1NC2=CC(=C(C=C2C1)OC)OCC1=CC=CC=C1
[N-]=[N+]=[N:23][C:5]([C:3]([O:2][CH3:1])=[O:4])=[CH:6][c:7]1[cH:8][c:9]([O:10][CH3:11])[c:12]([O:13][CH2:14][c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[cH:21][cH:22]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]2[cH:8][c:9]([O:10][CH3:11])[c:12]([O:13][CH2:14][c:15]3[cH:16][cH:17][cH:18][cH:19][cH:20]3)[cH:21][c:22]2[...
COC(=O)C(=Cc1ccc(OCc2ccccc2)c(OC)c1)N=[N+]=[N-]
COC(=O)c1cc2cc(OC)c(OCc3ccccc3)cc2[nH]1
null
null
C=1(C(=CC=CC1)C)C
Aromatic Heterocycle Formation
OtherReaction
edb9971602bfa0422050f727deecbcfa88df9e7fbb5c6b709e0e7c05fb641641
92e44103d9eed82e18506de89438be8bcf71f9d4943ea64c754ba56033058a29
c1ccc(COc2ccc3cc[nH]c3c2)cc1
[C;D1;H3:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[C;H0;D3;+0:5](=[CH;D2;+0:6]-[c:7](:[c:8]):[cH;D2;+0:9]:[c:10]:[c:11])-[N;H0;D2;+0:12]=[N+]=[N-]>>[C;D1;H3:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[c;H0;D3;+0:5]1:[cH;D2;+0:6]:[c:7](:[c:8]):[c;H0;D3;+0:9](:[c:10]:[c:11]):[nH;D2;+0:12]:1
null
[]
null
null
null
null
A solution of the azidocinnamate (55) (12.2 g, 36.0 mmol) prepared as described in example 247 in xylene (300 mL) was added dropwise to refluxing xylene (100 mL) over 1.5 h, the reaction mixture was heated at reflux for a further 15 min and then most of the xylene was removed by distillation. The residue, on cooling to...
10.6084/m9.figshare.5104873.v1
null
Ester.Azide
Ester
c1ccccc1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1
Other
C=1(C(=CC=CC1)C)C
null
null
COC(=O)C(=Cc1ccc(OCc2ccccc2)c(OC)c1)N=[N+]=[N-]>C=1(C(=CC=CC1)C)C>COC(=O)c1cc2cc(OC)c(OCc3ccccc3)cc2[nH]1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2762c7091e4841c693b05eddf337a72e
COC(=O)c1cc2cc(OC)c(OCc3ccccc3)cc2[nH]1>>COc1cc2cc(C=O)[nH]c2cc1OCc1ccccc1
[OH-].[Na+].COC(=O)C=1NC2=CC(=C(C=C2C1)OC)OCC1=CC=CC=C1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>>C(C1=CC=CC=C1)OC1=C(C=C2C=C(NC2=C1)C=O)OC
CO[C:8]([c:7]1[cH:6][c:5]2[cH:4][c:3]([O:2][CH3:1])[c:13]([O:14][CH2:15][c:16]3[cH:17][cH:18][cH:19][cH:20][cH:21]3)[cH:12][c:11]2[nH:10]1)=[O:9]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[cH:6][c:7]([CH:8]=[O:9])[nH:10][c:11]2[cH:12][c:13]1[O:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1
COC(=O)c1cc2cc(OC)c(OCc3ccccc3)cc2[nH]1
COc1cc2cc(C=O)[nH]c2cc1OCc1ccccc1
null
[O-2].[O-2].[Mn+4]
O1CCCC1
Reduction
OtherReaction
ec1c6c64dd9be73981e5a6c952ab740869d298b20e87e097e88e1179cc5bc6dc
33ddc7b9457742ba0a376f08a972e4f33779267f6f1fe15e3be786427ae9f4ec
c1ccc(COc2ccc3cc[nH]c3c2)cc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#7;a:5]:[c:6]>>[O;D1;H0:2]=[CH;D2;+0:1]-[c:3](:[c:4]):[#7;a:5]:[c:6]
82
[{"value": 82.0, "product": "C(C1=CC=CC=C1)OC1=C(C=C2C=C(NC2=C1)C=O)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 81.7, "product": "C(C1=CC=CC=C1)OC1=C(C=C2C=C(NC2=C1)C=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
To a solution of the ester (56) (1.0 g, 3.22 mmol) prepared as described in example 248 in tetrabydrofuran (10 mL) was added a suspension of lithium aluminum hydride (0.150 g, 3.86 mmol) in tetrahydrofuran (10 mL) dropwise, the reaction mixture was stirred at room temperature for 20 min. Water (1 mL) was added dropwise...
10.6084/m9.figshare.5104873.v1
null
Ester
Aldehyde
null
null
c1ccc2[nH]ccc2c1.c1ccccc1
HO-
[O-2].[O-2].[Mn+4].O1CCCC1
null
0.333333
COC(=O)c1cc2cc(OC)c(OCc3ccccc3)cc2[nH]1>[O-2].[O-2].[Mn+4].O1CCCC1>COc1cc2cc(C=O)[nH]c2cc1OCc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c4c6b20ef05246859197c01fa797a32d
COc1cc2cc(C=Cc3ccccc3Cl)[nH]c2cc1OCc1ccccc1.O=C1C=CC(=O)N1>>COc1cc2c3c([nH]c2cc1OCc1ccccc1)CC(c1ccccc1Cl)C1C(=O)NC(=O)C31
C(C1=CC=CC=C1)OC1=C(C=C2C=C(NC2=C1)C=CC1=C(C=CC=C1)Cl)OC.C1(C=CC(N1)=O)=O>>C(C1=CC=CC=C1)OC=1C(=CC=2C=3C4C(C(CC3NC2C1)C1=C(C=CC=C1)Cl)C(NC4=O)=O)OC
[CH3:1][O:2][c:3]1[cH:4][c:5]2[cH:6][c:7]([CH:20]=[CH:21][c:22]3[cH:23][cH:24][cH:25][cH:26][c:27]3[Cl:28])[nH:8][c:9]2[cH:10][c:11]1[O:12][CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1.[CH:29]1=[CH:35][C:33](=[O:34])[NH:32][C:30]1=[O:31]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]3[c:7]([nH:8][c:9]2[cH:10][c:11]1[O:12][...
COc1cc2cc(C=Cc3ccccc3Cl)[nH]c2cc1OCc1ccccc1.O=C1C=CC(=O)N1
COc1cc2c3c([nH]c2cc1OCc1ccccc1)CC(c1ccccc1Cl)C1C(=O)NC(=O)C31
null
null
null
C-C Coupling
OtherReaction
f4dfd9249675065a438272ee31ebbe56b42434dbbe67b7314944f01b1550fb32
410ec9b1cc243569e4ff568c248f0b402403802e002b4018f576af3f6960507b
O=C1NC(=O)C2C(c3ccccc3)Cc3[nH]c4cc(OCc5ccccc5)ccc4c3C12
[O;D1;H0:1]=[C:2]1-[#7:3]-[C:4](=[O;D1;H0:5])-[CH;D2;+0:6]=[CH;D2;+0:7]-1.[c:8]:[c:9]1:[#7;a:10]:[c:11](-[CH;D2;+0:12]=[CH;D2;+0:13]-[c:14](:[c:15]):[c:16]):[cH;D2;+0:17]:[c:18]:1:[c:19]>>[O;D1;H0:1]=[C:2]1-[#7:3]-[C:4](=[O;D1;H0:5])-[CH;D3;+0:6]2-[CH;D3;+0:7]-1-[CH;D3;+0:13](-[c:14](:[c:15]):[c:16])-[CH2;D2;+0:12]-[c:...
87
[{"value": 87.0, "product": "C(C1=CC=CC=C1)OC=1C(=CC=2C=3C4C(C(CC3NC2C1)C1=C(C=CC=C1)Cl)C(NC4=O)=O)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of the diene (155) prepared as described in example 255 with maleimide using the procedure described in example 69 gave the adduct (161) as a tan powder (87%), which was used without further purification. Conditions: See reaction.notes.procedure_details. Workup: prepared
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2[nH]ccc2c1.C1=CCNC1
c1ccc2c3c([nH]c2c1)CCC1CNCC31
c1ccccc1.c1ccccc1.c1ccc2c3c([nH]c2c1)CCC1CNCC31
null
null
null
null
COc1cc2cc(C=Cc3ccccc3Cl)[nH]c2cc1OCc1ccccc1.O=C1C=CC(=O)N1>>COc1cc2c3c([nH]c2cc1OCc1ccccc1)CC(c1ccccc1Cl)C1C(=O)NC(=O)C31
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d22ddd8026f748649d3dd6a766adff05
COc1cc2c3c([nH]c2cc1OCc1ccccc1)CC(c1ccccc1Cl)C1C(=O)NC(=O)C31>>COc1cc2c(cc1OCc1ccccc1)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
C(C1=CC=CC=C1)OC=1C(=CC=2C=3C4C(C(CC3NC2C1)C1=C(C=CC=C1)Cl)C(NC4=O)=O)OC>>C(C1=CC=CC=C1)OC=1C(=CC=2C=3C4=C(C(=CC3NC2C1)C1=C(C=CC=C1)Cl)C(NC4=O)=O)OC
[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[O:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[nH:17][c:18]1[c:30]2[CH:29]2[CH:28]([CH:20]([c:21]3[cH:22][cH:23][cH:24][cH:25][c:26]3[Cl:27])[CH2:19]1)[C:34](=[O:35])[NH:33][C:31]2=[O:32]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[O:9][CH2:10][c:11]1[cH:...
COc1cc2c3c([nH]c2cc1OCc1ccccc1)CC(c1ccccc1Cl)C1C(=O)NC(=O)C31
COc1cc2c(cc1OCc1ccccc1)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
null
[O-2].[O-2].[Mn+4]
null
Oxidation
OtherReaction
3d157ee1e52021ba4f102c0e4bf23d31153db03cc8f65d6ae2d3bbc53db1b830
82a3692de44364afcfd8cc4460435180e0752c31812bf6008d75e02664a32947
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3cc(OCc4ccccc4)ccc3c21
[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[CH;D3;+0:5]1-[CH2;D2;+0:6]-[c:7]2:[#7;a:8]:[c:9]:[c:10]:[c:11]:2-[CH;D3;+0:12]2-[C:13](=[O;D1;H0:14])-[#7:15]-[C:16](=[O;D1;H0:17])-[CH;D3;+0:18]-1-2):[c:19]:[c:20]>>[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[c;H0;D3;+0:5]1:[cH;D2;+0:6]:[c:7]2:[#7;a:8]:[c:9]:[c:10]:[c:11]:2:...
93
[{"value": 93.0, "product": "C(C1=CC=CC=C1)OC=1C(=CC=2C=3C4=C(C(=CC3NC2C1)C1=C(C=CC=C1)Cl)C(NC4=O)=O)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Aromatisation of (161) prepared as described in example 261 with manganese dioxide using the procedure described in example 79 gave the carbazole (162) (93%) as an orange powder, mp 260–264° C. 1H NMR δ [(CD3)2SO] 11.86 (s, 1H), 11.01 (s, 1H), 8.43 (s, 1H), 7.58–7.34 (m, 10H), 7.26 (s, 1H), 5.26 (s, 2H), 3.91 (s, 3H). ...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c3c([nH]c2c1)CCC1CNCC31
c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
c1ccccc1.c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
null
[O-2].[O-2].[Mn+4]
null
null
COc1cc2c3c([nH]c2cc1OCc1ccccc1)CC(c1ccccc1Cl)C1C(=O)NC(=O)C31>[O-2].[O-2].[Mn+4]>COc1cc2c(cc1OCc1ccccc1)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-44e17ed999e24f12a40be8ec409048b0
COc1ccc2cc(C=O)[nH]c2c1.c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1>>COc1ccc2cc(C=Cc3ccccc3)[nH]c2c1
COC1=CC=C2C=C(NC2=C1)C=O.[Br-].C(C1=CC=CC=C1)[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1>>COC1=CC=C2C=C(NC2=C1)C=CC1=CC=CC=C1
O=[CH:9][c:8]1[cH:7][c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:19][c:18]2[nH:17]1.c1ccc([P+](c2ccccc2)(c2ccccc2)[CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[cH:7][c:8]([CH:9]=[CH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][cH:16]3)[nH:17][c:18]2[cH:19]1
COc1ccc2cc(C=O)[nH]c2c1.c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
COc1ccc2cc(C=Cc3ccccc3)[nH]c2c1
null
null
null
C-C Coupling
Wittig with Phosphonium
cb5f277ac55a0e763ef643becc05f1522019cc4161daceb249ed2d634b78153b
cedc9d4b791e43eacf8e7ecfa6a98d1dc0438794e96e4f1c4bef436b78f82bd8
C(=Cc1cc2ccccc2[nH]1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[c:6]:[c:7](-[CH2;D2;+0:8]-[P+](-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1):[c:9]>>[c:6]:[c:7](-[CH;D2;+0:8]=[CH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5]):[c:9]
94
[{"value": 94.0, "product": "COC1=CC=C2C=C(NC2=C1)C=CC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of 6-methoxyindole-2-carboxaldehyde (145) with benzyltriphenylphosphonium bromide using the procedure described in example 37 gave (146) (94%) as a white solid (mixture of E/Z isomers) which was used without further purification. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aldehyde
null
c1ccccc1.c1ccccc1.c1ccccc1
null
c1ccc2[nH]ccc2c1.c1ccccc1
HO-
null
null
null
COc1ccc2cc(C=O)[nH]c2c1.c1ccc(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1>>COc1ccc2cc(C=Cc3ccccc3)[nH]c2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-48da5ed2f8704646a3a54504d181f110
N#CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O.[CH3][Sn]([CH3])([CH3])[N]=[N+]=[N-].[CH3][Sn]([CH3])([CH3])[N]=[N+]=[N-]>>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCc1nnn[nH]1
ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC#N.N(=[N+]=[N-])[Sn](C)(C)C.N(=[N+]=[N-])[Sn](C)(C)C>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC2=NN=NN2
[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[Cl:15])[cH:16][c:17]1[c:18]2[c:19]2[cH:20][c:21]([OH:22])[cH:23][cH:24][c:25]2[n:26]1[CH2:27][CH2:28][C:29]#[N:30].[CH3][Sn]([CH3])([CH3])[N:33]=[N+]=[N-].[CH3][Sn]([CH3])([CH3])[N:32]=[N+:31]=[N-]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5...
N#CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O.[CH3][Sn]([CH3])([CH3])[N]=[N+]=[N-].[CH3][Sn]([CH3])([CH3])[N]=[N+]=[N-]
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCc1nnn[nH]1
null
null
O.C(C)(=O)OCC.C1(=CC=CC=C1)C.CN(C=O)C
Aromatic Heterocycle Formation
OtherReaction
646c410a4d640a8a98513ee566d2532f14933769e7f019fbcabb087b4a016a35
d6a8817f429c74ff8b90214ce1b775ad05560db3c4a19d34769a0ffcc4046a33
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2ccccc2n1CCc1nnn[nH]1
[CH3]-[Sn](-[CH3])(-[CH3])-[N;H0;D2;+0:1]=[N+;H0;D2:2]=[N-].[CH3]-[Sn](-[CH3])(-[CH3])-[N;H0;D2;+0:3]=[N+]=[N-].[C:4]-[C:5]-[C;H0;D2;+0:6]#[N;H0;D1;+0:7]>>[C:4]-[C:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[n;H0;D2;+0:2]:[n;H0;D2;+0:1]:[nH;D2;+0:3]:1
72.2
[{"value": 72.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC2=NN=NN2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.2, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(NC2=O)=O)O)CCC2=NN=NN2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of nitrile (238) (0.68 g, 1.63 mmol) prepared as described in example 98 in toluene/dimethylformamide (5:1, 120 mL) was added azidotrimethyl tin (0.67 g, 3.26 mmol). The resulting solution was heated at reflux for 24 hours before a further portion of azidotrimethyl tin (0.34 g, 1.63 mmol) was added. After...
10.6084/m9.figshare.5104873.v1
null
Azide.Azide.Nitrile.Tin.Tin
null
null
c1nnn[nH]1
c1ccccc1.c1nnn[nH]1.C1NCc2c1ccc1nc3ccccc3c21
Sn
O.C(C)(=O)OCC.C1(=CC=CC=C1)C.CN(C=O)C
null
null
N#CCCn1c2ccc(O)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)NC3=O.[CH3][Sn]([CH3])([CH3])[N]=[N+]=[N-].[CH3][Sn]([CH3])([CH3])[N]=[N+]=[N-]>O.C(C)(=O)OCC.C1(=CC=CC=C1)C.CN(C=O)C>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1c2c2cc(O)ccc2n1CCc1nnn[nH]1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b5ff531db69c462a869d3c4a2037c1a7
COCC(O)Cn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O>>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CC(O)CO
OC(CN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)OC)COC>>OC(CN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O)CO
C[O:21][c:20]1[cH:19][c:18]2[c:17]3[c:6]4[c:7]([c:8](-[c:9]5[cH:10][cH:11][cH:12][cH:13][cH:14]5)[cH:15][c:16]3[n:25]([CH2:26][CH:27]([OH:28])[CH2:29][O:30]C)[c:24]2[cH:23][cH:22]1)[C:2](=[O:1])[NH:3][C:4]4=[O:5]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)[cH:15][c:16]...
COCC(O)Cn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O
O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CC(O)CO
null
null
C(C)(=O)OCC.CCCCCC
Deprotection
OtherReaction
4d6c8edd9fbb24fe93d1708ee72ea6d7f9f2ced9255486c584465734072583b3
0019c7eff1b5e27bd389d7453db70f02f82e6eb53fc11519e24abebafecd8503
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[C:2]-[C:3].C-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[C:2]-[OH;D1;+0:1].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]
31.6
[{"value": 31.0, "product": "OC(CN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O)CO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 31.6, "product": "OC(CN1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=CC=CC=C1)C(NC3=O)=O)O)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Demethylation of alcohol (225) (96 mg, 0.22 mmol) prepared as described in example 290 employing the procedure described in example 80 was followed by chromatography on silica eluting with ethyl acetate/hexane (4:1). Crystallisation from ethyl acetate/hexane gave phenol (226) (28 mg, 31%) as an orange/yellow powder, mp...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Primary alcohol.Aromatic alcohol
null
null
c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
Other
C(C)(=O)OCC.CCCCCC
null
null
COCC(O)Cn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4)cc21)C(=O)NC3=O>C(C)(=O)OCC.CCCCCC>O=C1NC(=O)c2c1c(-c1ccccc1)cc1c2c2cc(O)ccc2n1CC(O)CO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-18531f62cf63405188edd0bdbe1ede32
COc1ccc2[nH]c(C=Cc3ccccc3Cl)cc2c1.O=C1C=CC(=O)O1>>COc1ccc2[nH]c3c(c2c1)C1C(=O)OC(=O)C1C(c1ccccc1Cl)C3
ClC1=C(C=CC=C1)C=CC=1NC2=CC=C(C=C2C1)OC.C1(\C=C/C(=O)O1)=O>>ClC1=C(C=CC=C1)C1CC=2NC=3C=CC(=CC3C2C2C1C(OC2=O)=O)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]([CH:27]=[CH:19][c:20]3[cH:21][cH:22][cH:23][cH:24][c:25]3[Cl:26])[cH:9][c:10]2[cH:11]1.[CH:12]1=[CH:18][C:16](=[O:17])[O:15][C:13]1=[O:14]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]3[c:9]([c:10]2[cH:11]1)[CH:12]1[C:13](=[O:14])[O:15][C:16](=[O:17])[CH:18]1[CH:19]([c...
COc1ccc2[nH]c(C=Cc3ccccc3Cl)cc2c1.O=C1C=CC(=O)O1
COc1ccc2[nH]c3c(c2c1)C1C(=O)OC(=O)C1C(c1ccccc1Cl)C3
null
null
C=1(C(=CC=CC1)C)C
C-C Coupling
OtherReaction
e32df616349e641e98b0cb04d918a2f1c5ea561df38c6152b2e7436c0d681d1b
410ec9b1cc243569e4ff568c248f0b402403802e002b4018f576af3f6960507b
O=C1OC(=O)C2C(c3ccccc3)Cc3[nH]c4ccccc4c3C12
[O;D1;H0:1]=[C:2]1-[#8:3]-[C:4](=[O;D1;H0:5])-[CH;D2;+0:6]=[CH;D2;+0:7]-1.[c:8]:[c:9]1:[cH;D2;+0:10]:[c:11](-[CH;D2;+0:12]=[CH;D2;+0:13]-[c:14](:[c:15]):[c:16]):[#7;a:17]:[c:18]:1:[c:19]>>[O;D1;H0:1]=[C:2]1-[#8:3]-[C:4](=[O;D1;H0:5])-[CH;D3;+0:6]2-[CH;D3;+0:7]-1-[c;H0;D3;+0:10]1:[c:9](:[c:8]):[c:18](:[c:19]):[#7;a:17]:...
null
[]
null
null
null
null
A solution of trans-diene (27) (0.30 g, 1.06 mmol) prepared as described in example 37 and maleic anhydride (0.16 g, 1.59 mmol) in xylene (30 mL) were heated at reflux for 18 hours, before being concentrated in vacuo and chromatographed on silica eluting with ethyl acetatelhexane (1:2). Crystallisation from ethyl aceta...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2[nH]ccc2c1.C1=CCOC1
c1ccc2c3c([nH]c2c1)CCC1COCC31
c1ccccc1.c1ccc2c3c([nH]c2c1)CCC1COCC31
null
C=1(C(=CC=CC1)C)C
null
null
COc1ccc2[nH]c(C=Cc3ccccc3Cl)cc2c1.O=C1C=CC(=O)O1>C=1(C(=CC=CC1)C)C>COc1ccc2[nH]c3c(c2c1)C1C(=O)OC(=O)C1C(c1ccccc1Cl)C3
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-425a6fdd79984f919dc2fb2de7f6baed
COc1ccc(CN)c(OC)c1.COc1ccc2[nH]c3c(c2c1)C1C(=O)OC(=O)C1C(c1ccccc1Cl)C3>>COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1
ClC1=C(C=CC=C1)C1CC=2NC=3C=CC(=CC3C2C2C1C(OC2=O)=O)OC.COC1=C(CN)C=CC(=C1)OC>>ClC1=C(C=CC=C1)C1=CC=2NC=3C=CC(=CC3C2C2=C1C(N(C2=O)CC2=C(C=C(C=C2)OC)OC)=O)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][NH2:8])[c:35]([O:36][CH3:37])[cH:38]1.O1[C:9](=[O:10])[CH:11]2[CH:12]([c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[Cl:19])[CH2:20][c:21]3[nH:22][c:23]4[cH:24][cH:25][c:26]([O:27][CH3:28])[cH:29][c:30]4[c:31]3[CH:32]2[C:33]1=[O:34]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][N:...
COc1ccc(CN)c(OC)c1.COc1ccc2[nH]c3c(c2c1)C1C(=O)OC(=O)C1C(c1ccccc1Cl)C3
COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1
null
null
C(C)(=O)O
Acylation
OtherReaction
73046fde7b0f6328edcfd588f5c2e038ff2cc300c7e42ea70f46d7d4fe40722f
2a4a20e639c386292668b0b265a8e1b50d707d5f0576437dc5ade3e7fd444d29
O=C1c2c(-c3ccccc3)cc3[nH]c4ccccc4c3c2C(=O)N1Cc1ccccc1
[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[CH;D3;+0:5]1-[CH2;D2;+0:6]-[c:7]2:[#7;a:8]:[c:9]:[c:10]:[c:11]:2-[CH;D3;+0:12]2-[C;H0;D3;+0:13](=[O;D1;H0:14])-O-[C;H0;D3;+0:15](=[O;D1;H0:16])-[CH;D3;+0:17]-1-2):[c:18]:[c:19].[NH2;D1;+0:20]-[C:21]-[c:22]>>[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[c;H0;D3;+0:5]1:[cH;D2;+0:...
null
[]
null
null
null
null
To a solution of anhydride (286) (2.80 g, 7.42 mmol) prepared as described in example 296 in glacial acetic acid (70 mL) was added 2,4-dimethoxybenzylamine (1.67 mL, 11.1 mmol). The resulting solution was heated at reflux for 6 hours before being partially concentrated under reduced pressure and diluted with water to p...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Primary amine
Substituted dicarboximide
c1ccc2c3c([nH]c2c1)CCC1COCC31
c1ccc2c(c1)nc1ccc3c(c12)C[N]C3
c1ccccc1.c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)C[N]C3
HO-
C(C)(=O)O
null
null
COc1ccc(CN)c(OC)c1.COc1ccc2[nH]c3c(c2c1)C1C(=O)OC(=O)C1C(c1ccccc1Cl)C3>C(C)(=O)O>COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fd3a31722eab4427bb653cfb10123b6e
C=CCBr.COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1>>C=CCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O
ClC1=C(C=CC=C1)C1=CC=2NC=3C=CC(=CC3C2C2=C1C(N(C2=O)CC2=C(C=C(C=C2)OC)OC)=O)OC.C([O-])([O-])=O.[K+].[K+].C(C=C)Br>>C(C=C)N1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(N(C3=O)CC3=C(C=C(C=C3)OC)OC)=O)OC
Br[CH2:3][CH:2]=[CH2:1].[nH:4]1[c:5]2[cH:6][cH:7][c:8]([O:9][CH3:10])[cH:11][c:12]2[c:13]2[c:14]3[c:15]([c:16](-[c:17]4[cH:18][cH:19][cH:20][cH:21][c:22]4[Cl:23])[cH:24][c:25]12)[C:26](=[O:27])[N:28]([CH2:29][c:30]1[cH:31][cH:32][c:33]([O:34][CH3:35])[cH:36][c:37]1[O:38][CH3:39])[C:40]3=[O:41]>>[CH2:1]=[CH:2][CH2:3][n:...
C=CCBr.COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1
C=CCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O
null
null
C(C)(=O)OCC.O.CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
cddce2a874664e470793fc9c2c3968cab03ff58e8d853d30fd6a8d30bc88b7bf
4c606dc54eac846ef90c7b3255999ceff93277747e7c2b0ddd37ccf25562b7c5
O=C1c2c(-c3ccccc3)cc3[nH]c4ccccc4c3c2C(=O)N1Cc1ccccc1
Br-[CH2;D2;+0:1]-[C:2]=[C;D1;H2:3].[c:4]:[c:5]1:[c:6]:[c:7]:[c:8](:[c:9]):[nH;D2;+0:10]:1>>[C;D1;H2:3]=[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:10]1:[c:5](:[c:4]):[c:6]:[c:7]:[c:8]:1:[c:9]
57
[{"value": 57.0, "product": "C(C=C)N1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(N(C3=O)CC3=C(C=C(C=C3)OC)OC)=O)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 56.7, "product": "C(C=C)N1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(N(C3=O)CC3=C(C=C(C=C3)OC)OC)=O)OC", "details": "CALCULATEDPERCENTYIELD...
90
CELSIUS
3
HOUR
To a solution of carbazole (287) (150 mg, 0.28 mmol) prepared as described in example 297 in dimethylformamide (10 mL) under nitrogen was added potassium carbonate (0.39 g, 2.80 mmol) and allyl bromide (720L, 0.84 mmol). The resulting suspension was warmed to 90° C. with stirring for 3 hours before being diluted with w...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Allyl
Allyl
c1ccc2c(c1)[nH]c1ccc3c(c12)C[NH]C3
C1NCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21.c1ccccc1
HBr
C(C)(=O)OCC.O.CN(C=O)C
90
3
C=CCBr.COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1>C(C)(=O)OCC.O.CN(C=O)C>C=CCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-600ccf5b9b9540ba9a97d77d8ba42995
C=CCCBr.COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1>>C=CCCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O
ClC1=C(C=CC=C1)C1=CC=2NC=3C=CC(=CC3C2C2=C1C(N(C2=O)CC2=C(C=C(C=C2)OC)OC)=O)OC.BrCCC=C>>C(CC=C)N1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(N(C3=O)CC3=C(C=C(C=C3)OC)OC)=O)OC
Br[CH2:4][CH2:3][CH:2]=[CH2:1].[nH:5]1[c:6]2[cH:7][cH:8][c:9]([O:10][CH3:11])[cH:12][c:13]2[c:14]2[c:15]3[c:16]([c:17](-[c:18]4[cH:19][cH:20][cH:21][cH:22][c:23]4[Cl:24])[cH:25][c:26]12)[C:27](=[O:28])[N:29]([CH2:30][c:31]1[cH:32][cH:33][c:34]([O:35][CH3:36])[cH:37][c:38]1[O:39][CH3:40])[C:41]3=[O:42]>>[CH2:1]=[CH:2][C...
C=CCCBr.COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1
C=CCCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
9fdb054f006790672a590a47d7107803946a0e4d83da9b5f9c5cc6110c56f155
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=C1c2c(-c3ccccc3)cc3[nH]c4ccccc4c3c2C(=O)N1Cc1ccccc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3]=[C;D1;H2:4].[c:5]:[c:6]1:[c:7]:[c:8]:[c:9](:[c:10]):[nH;D2;+0:11]:1>>[C;D1;H2:4]=[C:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:11]1:[c:6](:[c:5]):[c:7]:[c:8]:[c:9]:1:[c:10]
58.4
[{"value": 58.0, "product": "C(CC=C)N1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(N(C3=O)CC3=C(C=C(C=C3)OC)OC)=O)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 58.4, "product": "C(CC=C)N1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(N(C3=O)CC3=C(C=C(C=C3)OC)OC)=O)OC", "details": "CALCULATEDPERCENTYIE...
null
null
null
null
Reaction of carbazole (287) (260 mg, 0.51 mmol) prepared as described in example 297 with 4-bromo-1-butene (155 □L, 1.53 mmol) according to procedure described in example 298 gave carbazole (289) (173 mg, 58%) as a yellow powder, mp 161–164° C. 1H NMR δ [(CD3)2SO] 8.50 (d, J=2.6 Hz, 1H), 7.89 (s, 1H), 7.73 (d, J=9.0 Hz...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1ccc2c(c1)[nH]c1ccc3c(c12)C[NH]C3
C1NCc2c1ccc1[nH]c3ccccc3c21
c1ccccc1.C1NCc2c1ccc1[nH]c3ccccc3c21.c1ccccc1
HBr
null
null
null
C=CCCBr.COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4[nH]c5ccc(OC)cc5c4c3C2=O)c(OC)c1>>C=CCCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f5196dcb4161474bbb05e2f36ea37b3b
C=CCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O.CC(C)=O.O>>COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4c(c3C2=O)c2cc(OC)ccc2n4CC(O)CO)c(OC)c1
C(C=C)N1C=2C=CC(=CC2C=2C3=C(C(=CC12)C1=C(C=CC=C1)Cl)C(N(C3=O)CC3=C(C=C(C=C3)OC)OC)=O)OC.C[N+]1(CCOCC1)[O-].CC(=O)C.O>>ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(N(C2=O)CC2=C(C=C(C=C2)OC)OC)=O)OC)CC(CO)O
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][N:8]2[C:9](=[O:10])[c:11]3[c:12](-[c:13]4[cH:14][cH:15][cH:16][cH:17][c:18]4[Cl:19])[cH:20][c:21]4[c:22]([c:23]3[C:24]2=[O:25])[c:26]2[cH:27][c:28]([O:29][CH3:30])[cH:31][cH:32][c:33]2[n:34]4[CH2:35][CH:36]=[CH2:38])[c:40]([O:41][CH3:42])[cH:43]1.CC(C)=[O:37].[OH2:39]>>[CH3:1...
C=CCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O.CC(C)=O.O
COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4c(c3C2=O)c2cc(OC)ccc2n4CC(O)CO)c(OC)c1
null
[Os](=O)(=O)(=O)=O
C(C)(=O)OCC.Cl
Heteroatom Alkylation and Arylation
OtherReaction
345506133277b562461fd4b28175e452202e676c1e8bfb3e7a07c6b5b46eb017
940633fa24d9f43cb0ba0036641980eb579ae4284341d810fa2427d9809d0d46
O=C1c2c(-c3ccccc3)cc3[nH]c4ccccc4c3c2C(=O)N1Cc1ccccc1
C-C(-C)=[O;H0;D1;+0:1].[#7;a:2]-[C:3]-[CH;D2;+0:4]=[CH2;D1;+0:5].[OH2;D0;+0:6]>>[#7;a:2]-[C:3]-[CH;D3;+0:4](-[OH;D1;+0:1])-[CH2;D2;+0:5]-[OH;D1;+0:6]
94
[{"value": 94.0, "product": "ClC1=C(C=CC=C1)C1=CC=2N(C=3C=CC(=CC3C2C2=C1C(N(C2=O)CC2=C(C=C(C=C2)OC)OC)=O)OC)CC(CO)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
To a solution of carbazole (288) (80 mg, 0.14 mmol) procedure described in example 298 in acetone/water (4:1, 20 mL) was added N-methylmorpholine N-oxide (33 mg, 0.28 mmol) and osmium tetroxide (176 uL, 4% solution in water, ˜0.028 mmol). The reaction mixture was stirred at room temperature for 18 hours before being di...
10.6084/m9.figshare.5104873.v1
null
Ketone.Allyl
Primary alcohol.Secondary alcohol
null
null
c1ccccc1.c1ccccc1.C1NCc2c1ccc1nc3ccccc3c21
Other
[Os](=O)(=O)(=O)=O.C(C)(=O)OCC.Cl
null
18
C=CCn1c2ccc(OC)cc2c2c3c(c(-c4ccccc4Cl)cc21)C(=O)N(Cc1ccc(OC)cc1OC)C3=O.CC(C)=O.O>[Os](=O)(=O)(=O)=O.C(C)(=O)OCC.Cl>COc1ccc(CN2C(=O)c3c(-c4ccccc4Cl)cc4c(c3C2=O)c2cc(OC)ccc2n4CC(O)CO)c(OC)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8fb542c851a94841addcbc8f675fb840
CCC[CH2][Sn](/[CH]=C/CCO)([CH2]CCC)[CH2]CCC.COc1cc2c(cc1OS(=O)(=O)C(F)(F)F)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O>>COc1cc2c(cc1/C=C/CCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
FC(S(=O)(=O)OC=1C(=CC=2C=3C4=C(C(=CC3NC2C1)C1=C(C=CC=C1)Cl)C(NC4=O)=O)OC)(F)F.C(CCC)[Sn](/C=C/CCO)(CCCC)CCCC.C(C)(=O)OCC.[Cl-].[Li+]>>ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)\C=C\CCO
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)/[CH:9]=[CH:10]/[CH2:11][CH2:12][OH:13].O=S(=O)(O[c:8]1[c:3]([O:2][CH3:1])[cH:4][c:5]2[c:6]([cH:7]1)[nH:14][c:15]1[cH:16][c:17](-[c:18]3[cH:19][cH:20][cH:21][cH:22][c:23]3[Cl:24])[c:25]3[c:26]([c:27]21)[C:28](=[O:29])[NH:30][C:31]3=[O:32])C(F)(F)F>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH...
CCC[CH2][Sn](/[CH]=C/CCO)([CH2]CCC)[CH2]CCC.COc1cc2c(cc1OS(=O)(=O)C(F)(F)F)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
COc1cc2c(cc1/C=C/CCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
null
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
CN(C)C=O
C-C Coupling
Stille reaction_other OTf
92ab09c73a964c1a0dcd7658e1a44c8859087c25093fbf9ea4d4c014f3f8cadd
46de4d1253710b3a7d4f46887df51b2ccba46e0a9427959558bd6f96ec8696eb
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-C-C-[CH2]-[Sn](-[CH2]-C-C-C)(-[CH2]-C-C-C)/[CH;D2;+0:1]=[C:2]/[C:3]-[C:4].F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:5]1:[c:6]:[c:7](:[#7;a:8]:[c:9]):[c:10]:[c:11]:[c:12]:1-[#8:13]>>[#8:13]-[c:12]1:[c:11]:[c:10]:[c:7](:[#7;a:8]:[c:9]):[c:6]:[c;H0;D3;+0:5]:1/[CH;D2;+0:1]=[C:2]/[C:3]-[C:4]
95.9
[{"value": 95.0, "product": "ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)\\C=C\\CCO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.9, "product": "ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)\\C=C\\CCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of the triflate (169) (0.20 g, 0.35 mmol) prepared as described in example 308, (3E)-4-(tributylstannyl)-3-buten-1-ol (0.19 g, 0.53 mmol) and lithium chloride (29 mg, 0.70 mmol) in DMF (10 mL) was purged by bubbling nitrogen through the liquid for 10 min. Bis(triphenylphosphine)palladium dichloride (12 mg, 0...
10.6084/m9.figshare.5104873.v1
null
Triflate.Tin
null
c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
TfOH.HO-.Sn
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.CN(C)C=O
null
null
CCC[CH2][Sn](/[CH]=C/CCO)([CH2]CCC)[CH2]CCC.COc1cc2c(cc1OS(=O)(=O)C(F)(F)F)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O>Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.CN(C)C=O>COc1cc2c(cc1/C=C/CCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5fdf3bedfc814e3c8a3029fbf4e6173c
COc1cc2c(cc1/C=C/CCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O>>COc1cc2c(cc1CCCCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)\C=C\CCO>>ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCO
[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1/[CH:9]=[CH:10]/[CH2:11][CH2:12][OH:13])[nH:14][c:15]1[cH:16][c:17](-[c:18]3[cH:19][cH:20][cH:21][cH:22][c:23]3[Cl:24])[c:25]3[c:26]([c:27]21)[C:28](=[O:29])[NH:30][C:31]3=[O:32]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[CH2:9][CH2:10][CH2:11][CH2:12][OH:13])[nH:1...
COc1cc2c(cc1/C=C/CCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
COc1cc2c(cc1CCCCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
null
O=[Pt]=O
O1CCCC1.CO
Reduction
Hydrogenation (double to single)
0bc3968b35f0839c230afb4215314da278abd4e1f10e42ec3012c5512de49ea5
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
[#7;a:1]:[c:2]:[c:3]:[c:4](/[CH;D2;+0:5]=[CH;D2;+0:6]/[C:7]-[C:8]):[c:9]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[C:7]-[C:8]):[c:9]
135
[{"value": 100.0, "product": "ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 135.0, "product": "ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A mixture of (170) (0.15 g, 0.33 mmol) prepared as described in example 309 and PtO2 (20 mg) in 1:1 tetrahydrofuran/methanol (30 mL) was shaken under an atmosphere of hydrogen gas at 40 psi pressure for 30 min. The catalyst was removed by filtration through Celite, washing through with more solvent. The combined filtra...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
null
O=[Pt]=O.O1CCCC1.CO
null
0.5
COc1cc2c(cc1/C=C/CCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O>O=[Pt]=O.O1CCCC1.CO>COc1cc2c(cc1CCCCO)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-aadb4706b7a04a7f8223ac521ce2756f
COc1cc2c(cc1CCCCOS(=O)(=O)C(F)(F)F)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O.[I-]>>COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
FC(S(=O)(=O)OCCCCC=1C(=CC=2C=3C4=C(C(=CC3NC2C1)C1=C(C=CC=C1)Cl)C(NC4=O)=O)OC)(F)F.[I-].[Na+]>>ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCI
O=S(=O)(O[CH2:12][CH2:11][CH2:10][CH2:9][c:8]1[c:3]([O:2][CH3:1])[cH:4][c:5]2[c:6]([cH:7]1)[nH:14][c:15]1[cH:16][c:17](-[c:18]3[cH:19][cH:20][cH:21][cH:22][c:23]3[Cl:24])[c:25]3[c:26]([c:27]21)[C:28](=[O:29])[NH:30][C:31]3=[O:32])C(F)(F)F.[I-:13]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[CH2:9][CH2:10][CH2:11][...
COc1cc2c(cc1CCCCOS(=O)(=O)C(F)(F)F)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O.[I-]
COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
null
null
C(C)(=O)OCC
Functional Group Interconversion
OtherReaction
8c25114f6e35a2eaed073de14ecf22ab2f1e189db18bca7f82e8c0b93444a0b1
23ab3c443e9999f7cd1707e344529116afaee675d7ed2bc5da5c5c7516fe5ad6
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
F-C(-F)(-F)-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[C:3].[I-;H0;D0:4]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[I;H0;D1;+0:4]
null
[]
null
null
null
null
A mixture of the mesylate (172) 0.12 g, 0.21 mmol) prepared as described in example 311 and sodium iodide (1 g) in ethyl acetate (50 mL) was refluxed for 4 h. The cooled solution was washed with water and worked up to give the iodide (173) which crystallised from tetrahydrofuran/petroleum ether as an orange powder (0.1...
10.6084/m9.figshare.5104873.v1
null
Triflate
Primary halide
null
null
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
TfOH
C(C)(=O)OCC
null
null
COc1cc2c(cc1CCCCOS(=O)(=O)C(F)(F)F)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O.[I-]>C(C)(=O)OCC>COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ef93ac7314bc40abb94057164ba9666f
CNC.COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O>>COc1cc2c(cc1CCCCN(C)C)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCI.CNC.COC1=CC=2C=3C4=C(C(=CC3NC2C=C1)C(=O)OCC1=CC=CC=C1)C(NC4=O)=O>>ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCN(C)C
[NH:13]([CH3:14])[CH3:15].I[CH2:12][CH2:11][CH2:10][CH2:9][c:8]1[c:3]([O:2][CH3:1])[cH:4][c:5]2[c:6]([cH:7]1)[nH:16][c:17]1[cH:18][c:19](-[c:20]3[cH:21][cH:22][cH:23][cH:24][c:25]3[Cl:26])[c:27]3[c:28]([c:29]21)[C:30](=[O:31])[NH:32][C:33]3=[O:34]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[CH2:9][CH2:10][CH2:11]...
CNC.COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
COc1cc2c(cc1CCCCN(C)C)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
6d58cac08ccced0a33ed16fbca180bc12aa011288d6476106d98a7b2cbc3d709
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
I-[CH2;D2;+0:1]-[C:2]-[C:3].[C;D1;H3:4]-[NH;D2;+0:5]-[C;D1;H3:6]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:5](-[C;D1;H3:4])-[C;D1;H3:6]
64
[{"value": 64.0, "product": "ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCN(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
6
HOUR
Reaction of the iodide (173) prepared as described in example 312 with aqueous dimethylamine using the procedure described in example 179 of Scheme 3 except that the reaction conditions were 6 h at room temperature gave (174) (64%) as an orange powder, mp 162–164° C. 1H NMR δ [(CD3)2SO] 11.85 (s, 1H), 11.04 (br s, 1H),...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
null
null
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
HI
null
null
6
CNC.COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O>>COc1cc2c(cc1CCCCN(C)C)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-53b8de3adf874b74b5aac8d0effc825e
C1CCNC1.COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O>>COc1cc2c(cc1CCCCN1CCCC1)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCI.N1CCCC1>>ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCN2CCCC2
[NH:13]1[CH2:14][CH2:15][CH2:16][CH2:17]1.I[CH2:12][CH2:11][CH2:10][CH2:9][c:8]1[c:3]([O:2][CH3:1])[cH:4][c:5]2[c:6]([cH:7]1)[nH:18][c:19]1[cH:20][c:21](-[c:22]3[cH:23][cH:24][cH:25][cH:26][c:27]3[Cl:28])[c:29]3[c:30]([c:31]21)[C:32](=[O:33])[NH:34][C:35]3=[O:36]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[CH2:9]...
C1CCNC1.COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
COc1cc2c(cc1CCCCN1CCCC1)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
19b442dc26882f89f7423416f5e0a16bdb8e48776df57991434a0634e21f0505
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3cc(CCCCN4CCCC4)ccc3c21
I-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]1-[C:5]-[C:6]-[C:7]-[NH;D2;+0:8]-1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:8]1-[C:4]-[C:5]-[C:6]-[C:7]-1
75
[{"value": 75.0, "product": "ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCN2CCCC2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
Reaction of the iodide (173) prepared as described in example 312 with pyrrolidine using the procedure described in example 179 except that the reaction conditions were 2 h at room temperature gave (176) (75%) as an orange powder, which was used without further purification, mp 173–178° C. 1H NMR δ [(CD3)2SO] 11.85 (s,...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNC1
C1CC[NH]C1
C1CC[NH]C1.c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
HI
null
null
2
C1CCNC1.COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O>>COc1cc2c(cc1CCCCN1CCCC1)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b586723b61704dd28d0ecfa2f449896d
COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O.c1ccncc1>>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1[nH]c3cc(CCCCN4CCCC4)c(O)cc3c21
ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)OC)CCCCI.Cl.N1=CC=CC=C1>>ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)O)CCCCN2CCCC2
C[O:32][c:31]1[c:21]([CH2:22][CH2:23][CH2:24][CH2:25]I)[cH:20][c:19]2[nH:18][c:17]3[cH:16][c:8](-[c:9]4[cH:10][cH:11][cH:12][cH:13][c:14]4[Cl:15])[c:7]4[c:6]([c:35]3[c:34]2[cH:33]1)[C:4](=[O:5])[NH:3][C:2]4=[O:1].c1[cH:27][n:26][cH:30][cH:29][cH:28]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:1...
COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O.c1ccncc1
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1[nH]c3cc(CCCCN4CCCC4)c(O)cc3c21
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
760b5eb134d6142f83c23e3407807f09fd7b138480e051dfde75d5bffde6bfc8
ed5750d8347e51bbb07e9a534b79c99e3dfd7c53478405edf0f6196ff85f5d14
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3cc(CCCCN4CCCC4)ccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].I-[CH2;D2;+0:5]-[C:6]-[C:7].[cH;D2;+0:8]1:[n;H0;D2;+0:9]:[cH;D2;+0:10]:[cH;D2;+0:11]:[cH;D2;+0:12]:c:1>>[C:7]-[C:6]-[CH2;D2;+0:5]-[N;H0;D3;+0:9]1-[CH2;D2;+0:8]-[CH2;D2;+0:12]-[CH2;D2;+0:11]-[CH2;D2;+0:10]-1.[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
72
[{"value": 72.0, "product": "ClC1=C(C=CC=C1)C1=CC=2NC=3C=C(C(=CC3C2C2=C1C(NC2=O)=O)O)CCCCN2CCCC2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Demethylation of (173) prepared as described in example 312 with pyridine hydrochloride using the procedure described in example 81 gave (177) (72%). 1H NMR δ [(CD3)2SO] 11.70 (s, 1H), 10.98 (br s, 1H), 9.30 (br, 1H), 8.31 (s, 1H), 7.57 (dd, J=8.0, 2.2 Hz, 1H), 7.49 (s, 1H), 7.49–7.40 (m, 3H), 7.32 (s, 1H), 2.73 (t, J=...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether
Aromatic alcohol.Tertiary amine
c1ccncc1
C1CC[NH]C1
c1ccccc1.c1ccc2c(c1)nc1ccc3c(c12)CNC3.C1CC[NH]C1
I-
null
null
null
COc1cc2c(cc1CCCCI)[nH]c1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O.c1ccncc1>>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1[nH]c3cc(CCCCN4CCCC4)c(O)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0431b74d082947e191c50707609c9568
COc1ccc2sc3cc(-c4ccccc4Cl)c4c(c3c2c1)C(=O)NC4=O>>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1sc3ccc(O)cc3c21
ClC1=C(C=CC=C1)C1=CC2=C(C=3C(NC(C13)=O)=O)C1=C(S2)C=CC(=C1)OC.B(Br)(Br)Br>>ClC1=C(C=CC=C1)C1=CC2=C(C=3C(NC(C13)=O)=O)C1=C(S2)C=CC(=C1)O
C[O:23][c:22]1[cH:21][cH:20][c:19]2[s:18][c:17]3[cH:16][c:8](-[c:9]4[cH:10][cH:11][cH:12][cH:13][c:14]4[Cl:15])[c:7]4[c:6]([c:26]3[c:25]2[cH:24]1)[C:4](=[O:5])[NH:3][C:2]4=[O:1]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[Cl:15])[cH:16][c:17]1[s:18][c:19]3[cH:20][cH:21][...
COc1ccc2sc3cc(-c4ccccc4Cl)c4c(c3c2c1)C(=O)NC4=O
O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1sc3ccc(O)cc3c21
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1sc3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
65
[{"value": 65.0, "product": "ClC1=C(C=CC=C1)C1=CC2=C(C=3C(NC(C13)=O)=O)C1=C(S2)C=CC(=C1)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
48
HOUR
Demethylation of (839) prepared as described in example 374 with BBr3 using the procedure described in example 80 except that the reaction time was 48 h gave (840) (65%) as a yellow solid, mp 311–313° C. 1H NMR δ [(CD3)2SO] 11.42 (s, 1H), 9.85 (s, 1H), 9.17 (d, J=2.5 Hz, 1H), 8.32 (s, 1H), 7.9 (d, J=9 Hz, 1H), 7.62 (m,...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.c1ccc2c(c1)sc1ccc3c(c12)CNC3
Other
null
null
48
COc1ccc2sc3cc(-c4ccccc4Cl)c4c(c3c2c1)C(=O)NC4=O>>O=C1NC(=O)c2c1c(-c1ccccc1Cl)cc1sc3ccc(O)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-449db22805af466fa07da83d9037e83d
CNC.COc1cc2c(cc1OCCCBr)oc1cc(-c3ccccc3Cl)c3c(c12)C(=O)N(CCCBr)C3=O>>COc1cc2c(cc1OCCCN(C)C)oc1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
BrCCCOC1=CC2=C(C=C1OC)C=1C=3C(N(C(C3C(=CC1O2)C2=C(C=CC=C2)Cl)=O)CCCBr)=O.CNC>>ClC1=C(C=CC=C1)C1=CC2=C(C=3C(NC(C13)=O)=O)C1=C(O2)C=C(C(=C1)OC)OCCCN(C)C
[NH:13]([CH3:14])[CH3:15].BrCCC[N:32]1[C:30](=[O:31])[c:28]2[c:27]([c:19](-[c:20]3[cH:21][cH:22][cH:23][cH:24][c:25]3[Cl:26])[cH:18][c:17]3[o:16][c:6]4[c:5]([cH:4][c:3]([O:2][CH3:1])[c:8]([O:9][CH2:10][CH2:11][CH2:12]Br)[cH:7]4)[c:29]32)[C:33]1=[O:34]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[O:9][CH2:10][CH2:1...
CNC.COc1cc2c(cc1OCCCBr)oc1cc(-c3ccccc3Cl)c3c(c12)C(=O)N(CCCBr)C3=O
COc1cc2c(cc1OCCCN(C)C)oc1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
OtherReaction
9a0cf426a88195917c644236d546ba744ba1149b5402e9c014f57ccddc78a4d1
8531a87128925ee84243b99e24583b0bc2fc05e7364ed3178245a169d9fe2986
O=C1NC(=O)c2c1c(-c1ccccc1)cc1oc3ccccc3c21
Br-C-C-C-[N;H0;D3;+0:1]1-[C:2](=[O;D1;H0:3])-[c:4]:[c:5]-[C:6]-1=[O;D1;H0:7].Br-[CH2;D2;+0:8]-[C:9]-[C:10].[C;D1;H3:11]-[NH;D2;+0:12]-[C;D1;H3:13]>>[C:10]-[C:9]-[CH2;D2;+0:8]-[N;H0;D3;+0:12](-[C;D1;H3:11])-[C;D1;H3:13].[O;D1;H0:3]=[C:2]1-[NH;D2;+0:1]-[C:6](=[O;D1;H0:7])-[c:5]:[c:4]-1
84
[{"value": 84.0, "product": "ClC1=C(C=CC=C1)C1=CC2=C(C=3C(NC(C13)=O)=O)C1=C(O2)C=C(C(=C1)OC)OCCCN(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
Reaction of dibromide (331) (100 mg, 0.16 mmol) prepared as described in example 385 with aqueous dimethylamine solution (40%, 5.0 mL) according to The procedure described in example 179, except that the reaction was performed in tetrahydrofuran (50 mL) at room temperature for 30 hours, gave the crude diamine (LXXX; Ar...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Substituted dicarboximide.Secondary amine
Unsubstituted dicarboximide.Tertiary amine
c1ccc2c(c1)oc1ccc3c(c12)C[NH]C3
c1ccc2c(c1)oc1ccc3c(c12)CNC3
c1ccccc1.c1ccc2c(c1)oc1ccc3c(c12)CNC3
HBr
O1CCCC1
null
24
CNC.COc1cc2c(cc1OCCCBr)oc1cc(-c3ccccc3Cl)c3c(c12)C(=O)N(CCCBr)C3=O>O1CCCC1>COc1cc2c(cc1OCCCN(C)C)oc1cc(-c3ccccc3Cl)c3c(c12)C(=O)NC3=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5a7efcaac9d44119a09dedaf3e502208
COc1ccc2[nH]c3c(C)c(-c4ccccc4)c4c(c3c2c1)C(=O)NC4=O>>Cc1c(-c2ccccc2)c2c(c3c1[nH]c1ccc(O)cc13)C(=O)NC2=O
COC1=CC=2C=3C4=C(C(=C(C3NC2C=C1)C)C1=CC=CC=C1)C(NC4=O)=O.B(Br)(Br)Br>>OC1=CC=2C=3C4=C(C(=C(C3NC2C=C1)C)C1=CC=CC=C1)C(NC4=O)=O
C[O:19][c:18]1[cH:17][cH:16][c:15]2[nH:14][c:13]3[c:2]([CH3:1])[c:3](-[c:4]4[cH:5][cH:6][cH:7][cH:8][cH:9]4)[c:10]4[c:11]([c:12]3[c:21]2[cH:20]1)[C:22](=[O:23])[NH:24][C:25]4=[O:26]>>[CH3:1][c:2]1[c:3](-[c:4]2[cH:5][cH:6][cH:7][cH:8][cH:9]2)[c:10]2[c:11]([c:12]3[c:13]1[nH:14][c:15]1[cH:16][cH:17][c:18]([OH:19])[cH:20][...
COc1ccc2[nH]c3c(C)c(-c4ccccc4)c4c(c3c2c1)C(=O)NC4=O
Cc1c(-c2ccccc2)c2c(c3c1[nH]c1ccc(O)cc13)C(=O)NC2=O
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1c(-c1ccccc1)cc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
90
[{"value": 90.0, "product": "OC1=CC=2C=3C4=C(C(=C(C3NC2C=C1)C)C1=CC=CC=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Demethylation of (803) prepared as described in example 406 with BBr3 using the procedure described in example 69 gave (804) (90%), mp 270–280° C. 1H NMR δ [(CD3)2SO] 11.60 (s, 1H), 10.82 (s, 1H), 9.22 (s, 1H), 8.31 (d, J=2.0 Hz, 1H), 7.47–7.42 (m, 4H), 7.36–7.23 (m, 2H), 7.06 (dd, J=8.7, 2.0 Hz, 1H), 2.32 (s, 3H). EIM...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
Other
null
null
null
COc1ccc2[nH]c3c(C)c(-c4ccccc4)c4c(c3c2c1)C(=O)NC4=O>>Cc1c(-c2ccccc2)c2c(c3c1[nH]c1ccc(O)cc13)C(=O)NC2=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9bcf57638ec4461986b37612b541e68c
COc1ccc2[nH]c(C=O)cc2c1.[Br][Mg][c]1ccccc1>>COc1ccc2[nH]c(C(=O)c3ccccc3)cc2c1
COC=1C=C2C=C(NC2=CC1)C=O.C1(=CC=CC=C1)[Mg]Br>>COC=1C=C2C=C(NC2=CC1)C(=O)C1=CC=CC=C1
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]([CH:9]=[O:10])[cH:17][c:18]2[cH:19]1.[Br][Mg][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]([C:9](=[O:10])[c:11]3[cH:12][cH:13][cH:14][cH:15][cH:16]3)[cH:17][c:18]2[cH:19]1
COc1ccc2[nH]c(C=O)cc2c1.[Br][Mg][c]1ccccc1
COc1ccc2[nH]c(C(=O)c3ccccc3)cc2c1
null
null
null
C-C Coupling
OtherReaction
813a2aef5e31d204b1b98b796e22e80eaacaf5654877ef9187d7a6f9ad0ac4fe
7db11402b2132cd2d08e947c3439b66a3e13f302984dbd7579c68a04c5d289a9
O=C(c1ccccc1)c1cc2ccccc2[nH]1
[Br]-[Mg]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[O;D1;H0:6]=[CH;D2;+0:7]-[c:8](:[c:9]):[#7;a:10]:[c:11]>>[O;D1;H0:6]=[C;H0;D3;+0:7](-[c:8](:[c:9]):[#7;a:10]:[c:11])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
91
[{"value": 91.0, "product": "COC=1C=C2C=C(NC2=CC1)C(=O)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction of 5-methoxy-1H-indole-2-carbaldehyde with phenylmagnesium bromide using the procedure described in example 404 gave (805) (91%), mp 159–161° C. 1H NMR δ [(CD3)2SO] 11.86 (s, 1H), 7.94–7.91 (m, 2H), 7.71–7.66 (m, 1H), 7.61–7.57 (m, 2H), 7.42 (d, J=8.9 Hz, 1H), 7.16 (d, J=2.4 Hz, 1H), 7.03 (s, 1H), 6.99 (dd, J=...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Aldehyde
Ketone
c1ccccc1
c1ccccc1
c1ccc2[nH]ccc2c1.c1ccccc1
HBr.Mg
null
null
null
COc1ccc2[nH]c(C=O)cc2c1.[Br][Mg][c]1ccccc1>>COc1ccc2[nH]c(C(=O)c3ccccc3)cc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5b1bf34dd4f9437a87340eb2f2be19a6
COc1ccc2[nH]c3ccc4c(c3c2c1)C(=O)NC4=O>>O=C1NC(=O)c2c1ccc1[nH]c3ccc(O)cc3c21
COC1=CC=2C=3C4=C(C=CC3NC2C=C1)C(NC4=O)=O.B(Br)(Br)Br>>OC1=CC=2C=3C4=C(C=CC3NC2C=C1)C(NC4=O)=O
C[O:16][c:15]1[cH:14][cH:13][c:12]2[nH:11][c:10]3[cH:9][cH:8][c:7]4[c:6]([c:19]3[c:18]2[cH:17]1)[C:4](=[O:5])[NH:3][C:2]4=[O:1]>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[c:6]2[c:7]1[cH:8][cH:9][c:10]1[nH:11][c:12]3[cH:13][cH:14][c:15]([OH:16])[cH:17][c:18]3[c:19]21
COc1ccc2[nH]c3ccc4c(c3c2c1)C(=O)NC4=O
O=C1NC(=O)c2c1ccc1[nH]c3ccc(O)cc3c21
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1NC(=O)c2c1ccc1[nH]c3ccccc3c21
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
79
[{"value": 79.0, "product": "OC1=CC=2C=3C4=C(C=CC3NC2C=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Demethylation of (816) prepared as described in example 416 with BBr3 using the procedure described in example 80 gave (817) (79%), mp 335–345° C. 1H NMR δ [(CD3)2SO] 11.77 (s, 1H), 11.04 (s, 1H), 9.23 (s, 1H), 8.24 (d, J=2.3 Hz, 1H), 7.75 (2d, J=8.2 Hz, 2H), 7.43 (d, J=8.7 Hz, 1H), 7.05 (dd, J=8.7, 2.3 Hz, 1H). Found:...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccc2c(c1)nc1ccc3c(c12)CNC3
Other
null
null
null
COc1ccc2[nH]c3ccc4c(c3c2c1)C(=O)NC4=O>>O=C1NC(=O)c2c1ccc1[nH]c3ccc(O)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e7283af0700a4001ac72fdbb3ed5f745
C=C(c1ccccc1)c1cc2cc(OC)ccc2[nH]1.O=C1C=CC(=O)N1>>COc1ccc2[nH]c3c(-c4ccccc4)cc4c(c3c2c1)C(=O)NC4=O
C1(=CC=CC=C1)C(=C)C=1NC2=CC=C(C=C2C1)OC.C1(C=CC(N1)=O)=O>>COC1=CC=2C=3C4=C(C=C(C3NC2C=C1)C1=CC=CC=C1)C(NC4=O)=O
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]([C:9]([c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)=[CH2:16])[cH:19][c:20]2[cH:21]1.[CH:17]1=[CH:18][C:22](=[O:23])[NH:24][C:25]1=[O:26]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[nH:7][c:8]3[c:9](-[c:10]4[cH:11][cH:12][cH:13][cH:14][cH:15]4)[cH:16][c:17]4[c:18]([c:19]3[c:20]2[...
C=C(c1ccccc1)c1cc2cc(OC)ccc2[nH]1.O=C1C=CC(=O)N1
COc1ccc2[nH]c3c(-c4ccccc4)cc4c(c3c2c1)C(=O)NC4=O
null
null
null
Miscellaneous
OtherReaction
8fd53892c6f95a0a445846d9674be0e26fba6bf545b8b38fd5a439008db94b85
62104ffcb4d4ab6482284e0c7ae124bc1d1d4f4befe80d570c6848ac4dc98f52
O=C1NC(=O)c2c1cc(-c1ccccc1)c1[nH]c3ccccc3c21
[CH2;D1;+0:1]=[C;H0;D3;+0:2](-[c:3]1:[#7;a:4]:[c:5](:[c:6]):[c:7](:[c:8]):[cH;D2;+0:9]:1)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14].[O;D1;H0:15]=[C:16]1-[#7:17]-[C:18](=[O;D1;H0:19])-[CH;D2;+0:20]=[CH;D2;+0:21]-1>>[O;D1;H0:15]=[C:16]1-[#7:17]-[C:18](=[O;D1;H0:19])-[c;H0;D3;+0:20]2:[cH;D2;+0:1]:[c;H0;D3;+0:2](-[c;H0...
73
[{"value": 73.0, "product": "COC1=CC=2C=3C4=C(C=C(C3NC2C=C1)C1=CC=CC=C1)C(NC4=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
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null
Reaction of (818) prepared as described in example 418 with maleimide at 180° C. using the procedure described in example 69 gave the adduct (XCVIII; R=phenyl, R′═H) (819), which was used without further purification. The crude Diels-Alder adduct was aromatised with MnO2 using the procedure described in example 79 to g...
10.6084/m9.figshare.5104873.v1
null
Vinyl
null
c1ccc2[nH]ccc2c1.C1=CCNC1
c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
c1ccccc1.c1ccc2c(c1)[nH]c1ccc3c(c12)CNC3
null
null
null
null
C=C(c1ccccc1)c1cc2cc(OC)ccc2[nH]1.O=C1C=CC(=O)N1>>COc1ccc2[nH]c3c(-c4ccccc4)cc4c(c3c2c1)C(=O)NC4=O