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
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14
3.37k
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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
time_units
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-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-f5ef483caa0240adbbfeffbf134b4a0e
CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)OC(C)(C)C>>CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1
I[Si](C)(C)C.C(C)(C)(C)OC(=O)N1C(SC[C@H]1C(=O)OC(C)(C)C)CC1=CC=CC=C1.O>>C(C1=CC=CC=C1)C1SC[C@H](N1)C(=O)OC(C)(C)C
CC(C)(C)OC(=O)[N:19]1[C@H:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][S:10][CH:11]1[CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@@H:8]1[CH2:9][S:10][CH:11]([CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[NH:19]1
CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)OC(C)(C)C
CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1
null
null
C(Cl)(Cl)Cl
Reduction
Boc amine deprotection
f43a6818a2dad1b74fffb8578c65ec32e6a9ffddc1d934cb7e8e04a9995976d0
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc(CC2NCCS2)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2](-[C:3])-[#16:4]-[C:5]-[C:6]-1-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C;D1;H3:13]>>[C:3]-[C:2]1-[#16:4]-[C:5]-[C:6](-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C;D1;H3:13])-[NH;D2;+0:1]-1
111.3
[{"value": 111.3, "product": "C(C1=CC=CC=C1)C1SC[C@H](N1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
C tert-Butyl (2RS,4R)-2-benzyl-4-thiazolidinecarboxalate may be prepared in the following 11.8 cm3 of iodotrimethyl-silane are introduced slowly at a temperature in the region of 25° C. into a solution of 30.5 g of tert-butyl (4R)-3-tert-butoxycarbonyl-2-benzyl-4-thiazolidine-carboxylate (isomer A) in 250 cm3 of chloro...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CSC[NH]1
C1CSCN1
C1CSCN1.c1ccccc1
HO-
C(Cl)(Cl)Cl
null
1
CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)OC(C)(C)C>C(Cl)(Cl)Cl>CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-0864c7b521d14d7eb031a94545d74b0f
O=C(O)C1CSC(Cc2ccccc2)N1>>O=C(O)[C@@H]1CSC(Cc2ccccc2)N1
C1(=CC=CC=C1)CC=O.C(C1=CC=CC=C1)C1SCC(N1)C(=O)O.N[C@@H](CS)C(=O)O>>C(C1=CC=CC=C1)C1SC[C@H](N1)C(=O)O
[O:1]=[C:2]([OH:3])[CH:4]1[CH2:5][S:6][CH:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[NH:15]1>>[O:1]=[C:2]([OH:3])[C@@H:4]1[CH2:5][S:6][CH:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[NH:15]1
O=C(O)C1CSC(Cc2ccccc2)N1
O=C(O)[C@@H]1CSC(Cc2ccccc2)N1
null
null
null
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(CC2NCCS2)cc1
null
null
[]
null
null
null
null
F (2RS, 4R) -2-Benzyl-4-thiazolidinecarboxylic acid may be prepared in a manner similar to that described in Example 1E, but starting with 53.7 g of L-cysteine and 56.5 g of phenylacetaldehyde. 75.8 g of (2RS,4R)-2-benzyl-4-thiazolidinecarboxylic acid, melting point 200° C., are thereby obtained. Conditions: See reacti...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
C1CSCN1.c1ccccc1
null
null
null
null
O=C(O)C1CSC(Cc2ccccc2)N1>>O=C(O)[C@@H]1CSC(Cc2ccccc2)N1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ffb54698da8d46458dc9823e743c6180
CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1>>CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)CC1=CC=CC=C1)C(CNC(NC=1C=C(C=CC1)CC(=O)OCC1=CC=CC=C1)=O)=O.C(=O)[O-].[NH4+]>>C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)CC1=CC=CC=C1)C(CNC(NC=1C=C(C=CC1)CC(=O)O)=O)=O
c1ccc(C[O:35][C:33]([CH2:32][c:31]2[cH:30][cH:29][cH:28][c:27]([NH:26][C:24]([NH:23][CH2:22][C:20]([N:19]3[C@H:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][S:10][CH:11]3[CH2:12][c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)=[O:21])=[O:25])[cH:36]2)=[O:34])cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7...
CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1
CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
null
[Pd]
null
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C(NCC(=O)N1CCSC1Cc1ccccc1)Nc1ccccc1
[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]
48.3
[{"value": 48.3, "product": "C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)CC1=CC=CC=C1)C(CNC(NC=1C=C(C=CC1)CC(=O)O)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The procedure is similar to that described in Example 1, but starting with 2.58 g of benzyl (4R)-3-{3-[2-(4-tert-butoxycarbonyl-2-benzyl-3-thiazolidinyl)-2-oxoethyl]ureido}phenylacetate (isomer A) , 1.6 g of ammonium formate and 1.3 g of palladium on charcoal (10% Pd). 1.06 g of (4R) -3-{3-[2-(4-tert-butoxycarbonyl-2-b...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
C1CSC[NH]1.c1ccccc1.c1ccccc1
Other
[Pd]
null
null
CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1>[Pd]>CC(C)(C)OC(=O)[C@@H]1CSC(Cc2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-e2c9b42b51d54157a9085a6f40b8120e
COC(=O)Cc1cccc(NC(=O)NCC(=O)N2C(C3CC4C=CC3C4)SC[C@H]2C(=O)OC(C)(C)C)c1>>CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)C1C2C=CC(C1)C2)C(CNC(NC=2C=C(C=CC2)CC(=O)OC)=O)=O.[OH-].[K+]>>C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)C1C2C=CC(C1)C2)C(CNC(NC=2C=C(C=CC2)CC(=O)O)=O)=O
C[O:35][C:33]([CH2:32][c:31]1[cH:30][cH:29][cH:28][c:27]([NH:26][C:24]([NH:23][CH2:22][C:20]([N:19]2[C@H:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][S:10][CH:11]2[CH:12]2[CH2:13][CH:14]3[CH:15]=[CH:16][CH:17]2[CH2:18]3)=[O:21])=[O:25])[cH:36]1)=[O:34]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@...
COC(=O)Cc1cccc(NC(=O)NCC(=O)N2C(C3CC4C=CC3C4)SC[C@H]2C(=O)OC(C)(C)C)c1
CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
null
null
null
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C(NCC(=O)N1CCSC1C1CC2C=CC1C2)Nc1ccccc1
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
5.1
[{"value": 5.1, "product": "C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)C1C2C=CC(C1)C2)C(CNC(NC=2C=C(C=CC2)CC(=O)O)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The procedure is as in Example 4, but starting with 0.6 g of methyl (4R)-3-[3-{2-[4-tert-butoxycarbonyl-2-[(2RS)-5-norbornen-2-yl]-3-thiazolidinyl]-2-oxoethyl}ureido]phenylacetate (mixture of isomers C and D) and 0.074 g of potassium hydroxide. 0.03 g of (4R) -3- [3-{2-[4-tert-butoxycarbonyl-2-[(2RS) -5-norbornen-2-yl]...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CSC[NH]1.C1=CC2CCC1C2.c1ccccc1
Other
null
null
null
COC(=O)Cc1cccc(NC(=O)NCC(=O)N2C(C3CC4C=CC3C4)SC[C@H]2C(=O)OC(C)(C)C)c1>>CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-73543e7f76764526bdad67044d707af0
CC(C)(C)OC(=O)NCC(=O)N1C(C2CC3C=CC2C3)SC[C@H]1C(=O)OC(C)(C)C>>CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CN
C12C(CC(C=C1)C2)C2SCC(N2)C(=O)[O-].C(C)(C)(C)OC(=O)NCC(=O)N1C(SC[C@H]1C(=O)OC(C)(C)C)C1C2C=CC(C1)C2.I[Si](C)(C)C>>NCC(=O)N1C(SC[C@H]1C(=O)OC(C)(C)C)C1C2C=CC(C1)C2
CC(C)(C)OC(=O)[NH:23][CH2:22][C:20]([N:19]1[C@H:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][S:10][CH:11]1[CH:12]1[CH2:13][CH:14]2[CH:15]=[CH:16][CH:17]1[CH2:18]2)=[O:21]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@@H:8]1[CH2:9][S:10][CH:11]([CH:12]2[CH2:13][CH:14]3[CH:15]=[CH:16][CH:17]2[CH2:18]...
CC(C)(C)OC(=O)NCC(=O)N1C(C2CC3C=CC2C3)SC[C@H]1C(=O)OC(C)(C)C
CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CN
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
C1=CC2CC1CC2C1NCCS1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3](=[O;D1;H0:4])-[#7:5](-[C:6]-[#16:7])-[C:8]-[C:9](-[#8:10])=[O;D1;H0:11]>>[#16:7]-[C:6]-[#7:5](-[C:3](=[O;D1;H0:4])-[C:2]-[NH2;D1;+0:1])-[C:8]-[C:9](-[#8:10])=[O;D1;H0:11]
99.8
[{"value": 99.8, "product": "NCC(=O)N1C(SC[C@H]1C(=O)OC(C)(C)C)C1C2C=CC(C1)C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
tert-Butyl (4R)-3-2-aminoacetyl)-2-[(2RS)-5-norbornen-2-yl]-4-thiazolidinecarboxylate (mixture of isomers C and D) may be prepared in a manner similar to that described in Example 1B, but starting with 1.0 g of tert-butyl (4R)-3-(2-tert-butoxycarbonylaminoacetyl)-2-[(2RS)-5-norbornen-2-yl]-4-thiazolidinecarboxylate (mi...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CSC[NH]1.C1=CC2CCC1C2
HO-
null
null
null
CC(C)(C)OC(=O)NCC(=O)N1C(C2CC3C=CC2C3)SC[C@H]1C(=O)OC(C)(C)C>>CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CN
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-e052a83f32a340ebb3ba8deb4770dd4e
CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1>>CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3CCC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)C1C2C=CC(C1)C2)C(CNC(NC=2C=C(C=CC2)CC(=O)OCC2=CC=CC=C2)=O)=O.C(=O)[O-].[NH4+]>>C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)C1C2CCC(C1)C2)C(CNC(NC=2C=C(C=CC2)CC(=O)O)=O)=O
c1ccc(C[O:35][C:33]([CH2:32][c:31]2[cH:30][cH:29][cH:28][c:27]([NH:26][C:24]([NH:23][CH2:22][C:20]([N:19]3[C@H:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][S:10][CH:11]3[CH:12]3[CH2:13][CH:14]4[CH:15]=[CH:16][CH:17]3[CH2:18]4)=[O:21])=[O:25])[cH:36]2)=[O:34])cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](...
CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1
CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3CCC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
null
[Pd]
null
Deprotection
OtherReaction
751cb6466f215f44096f47e9cfe8ba7ab9f935cb00f844009e88b83819ca32d7
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C(NCC(=O)N1CCSC1C1CC2CCC1C2)Nc1ccccc1
[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1.[C:5]1-[C:6]-[C:7]2-[C:8]-[C:9]-1-[CH;D2;+0:10]=[CH;D2;+0:11]-2>>[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4].[C:5]1-[C:6]-[C:7]2-[C:8]-[C:9]-1-[CH2;D2;+0:10]-[CH2;D2;+0:11]-2
41
[{"value": 41.0, "product": "C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)C1C2CCC(C1)C2)C(CNC(NC=2C=C(C=CC2)CC(=O)O)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The procedure is as in Example 1, but starting with 0.2 g of benzyl (4R)-3-[3-{2-[4-tert-butoxycarbonyl-2-[(2RS)-5-norbornen-2-yl]-3-thiazolidinyl]-2-oxoethyl}ureido]phenylacetate (mixture of isomers C and D), 0.13 g of Ammonium formate and 0.2 g of palladium on charcoal (10% Pd). 0.07 g of (4R)-3-[3-{2-[4-tert-butoxyc...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
C1=CC2CCC1C2.c1ccccc1
C1CC2CCC1C2
C1CSC[NH]1.C1CC2CCC1C2.c1ccccc1
Other
[Pd]
null
null
CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3C=CC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1>[Pd]>CC(C)(C)OC(=O)[C@@H]1CSC(C2CC3CCC2C3)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-4bc9a35c6a6d473b92f6f84258e723b3
CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CN.Cc1cccc(N=C=O)c1>>CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C)c1
NCC(=O)N1C(SC[C@H]1C(=O)OC(C)(C)C)CCCC.CC=1C=C(C=CC1)N=C=O>>CC=1C=C(C=CC1)NC(NCC(=O)N1C(SC[C@H]1C(=O)OC(C)(C)C)CCCC)=O
[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]1[S:6][CH2:7][C@@H:8]([C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15])[N:16]1[C:17](=[O:18])[CH2:19][NH2:20].[C:21](=[O:22])=[N:23][c:24]1[cH:25][cH:26][cH:27][c:28]([CH3:29])[cH:30]1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]1[S:6][CH2:7][C@@H:8]([C:9](=[O:10])[O:11][C:12]([CH3:13])([...
CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CN.Cc1cccc(N=C=O)c1
CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C)c1
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCC(=O)N1CCSC1)Nc1ccccc1
[#16:1]-[C:2]-[#7:3](-[C:4](=[O;D1;H0:5])-[C:6]-[NH2;D1;+0:7])-[C:8]-[C:9](-[#8:10])=[O;D1;H0:11].[O;D1;H0:12]=[C;H0;D2;+0:13]=[N;H0;D2;+0:14]-[c:15](:[c:16]):[c:17]>>[#16:1]-[C:2]-[#7:3](-[C:4](=[O;D1;H0:5])-[C:6]-[NH;D2;+0:7]-[C;H0;D3;+0:13](=[O;D1;H0:12])-[NH;D2;+0:14]-[c:15](:[c:16]):[c:17])-[C:8]-[C:9](-[#8:10])=[...
46.3
[{"value": 46.3, "product": "CC=1C=C(C=CC1)NC(NCC(=O)N1C(SC[C@H]1C(=O)OC(C)(C)C)CCCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The procedure is similar to that described in Example 1A, but starting with 1.2 g of tert-butyl (4R)-3-(2-aminoacetyl)-2-butyl-4-thiazolidinecarboxylate (isomer A) and 0.53 g of 3-methylphenyl isocyanate. The crude product is purified by chromatography on silica [eluent: diisopropyl ether/ethyl acetate (95:5 by volume)...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
C1CSC[NH]1.c1ccccc1
null
null
null
null
CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CN.Cc1cccc(N=C=O)c1>>CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C)c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-e00d18b187a74148a66e17d1bf97c616
CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C(=O)OCc2ccccc2)c1>>CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C(=O)O)c1
C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)CCCC)C(CNC(NC=1C=C(C(=O)OCC2=CC=CC=C2)C=CC1)=O)=O.C(=O)[O-].[NH4+]>>C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)CCCC)C(CNC(NC=1C=C(C(=O)O)C=CC1)=O)=O
c1ccc(C[O:31][C:29]([c:28]2[cH:27][cH:26][cH:25][c:24]([NH:23][C:21]([NH:20][CH2:19][C:17]([N:16]3[CH:5]([CH2:4][CH2:3][CH2:2][CH3:1])[S:6][CH2:7][C@H:8]3[C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15])=[O:18])=[O:22])[cH:32]2)=[O:30])cc1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]1[S:6][CH2:7][C@@H:8]([C:9](=[O:10])[O:...
CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C(=O)OCc2ccccc2)c1
CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C(=O)O)c1
null
[Pd]
CN(C)C=O
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C(NCC(=O)N1CCSC1)Nc1ccccc1
[O;D1;H0:1]=[C:2](-[c:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[O;D1;H0:1]=[C:2](-[OH;D1;+0:4])-[c:3]
25.3
[{"value": 25.3, "product": "C(C)(C)(C)OC(=O)[C@H]1N(C(SC1)CCCC)C(CNC(NC=1C=C(C(=O)O)C=CC1)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The procedure is similar to that described in Example 1, but starting with 1.18 g of benzyl (4R)-3-{3-[2-(4-tert-butoxycarbonyl-2-butyl-3-thiazolidinyl)-2-oxoethyl]ureido}benzoate (isomer A), 0.8 g of ammonium formate and 1.2 g of palladium on charcoal (10% Pd). 0.25 g of (4R) -3-{3- [2- (4-tert-butoxycarbonyl-2-butyl-...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
C1CSC[NH]1.c1ccccc1
Other
[Pd].CN(C)C=O
null
null
CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C(=O)OCc2ccccc2)c1>[Pd].CN(C)C=O>CCCCC1SC[C@@H](C(=O)OC(C)(C)C)N1C(=O)CNC(=O)Nc1cccc(C(=O)O)c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-b47779451583489f80b26bac401c4f5d
CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1>>CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
C(C)(C)(C)OC(=O)[C@H]1N([C@H](SC1)C1=C(C=CC=C1)C1=CC=CC=C1)C(CNC(NC=1C=C(C=CC1)CC(=O)OCC1=CC=CC=C1)=O)=O.C(=O)[O-].[NH4+]>>C(C)(C)(C)OC(=O)[C@H]1N([C@H](SC1)C1=C(C=CC=C1)C1=CC=CC=C1)C(CNC(NC=1C=C(C=CC1)CC(=O)O)=O)=O
c1ccc(C[O:40][C:38]([CH2:37][c:36]2[cH:35][cH:34][cH:33][c:32]([NH:31][C:29]([NH:28][CH2:27][C:25]([N:24]3[C@H:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][S:10][C@@H:11]3[c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3-[c:18]3[cH:19][cH:20][cH:21][cH:22][cH:23]3)=[O:26])=[O:30])[cH:41]2)=[O:39])cc1>>[CH3:1][C...
CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1
CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
null
[Pd]
null
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C(NCC(=O)N1CCS[C@@H]1c1ccccc1-c1ccccc1)Nc1ccccc1
[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]
21.3
[{"value": 21.3, "product": "C(C)(C)(C)OC(=O)[C@H]1N([C@H](SC1)C1=C(C=CC=C1)C1=CC=CC=C1)C(CNC(NC=1C=C(C=CC1)CC(=O)O)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The procedure is similar to that described in Example 1, but starting with 1.36 g of benzyl (2R,4R)-3-[3-{2-[4-tert-butoxycarbonyl-2-(2-phenylphenyl)-3-thiazolidinyl]-2-oxoethyl}ureido]phenylacetate, 0.44 g of ammonium formate and 0.6 g of palladium on charcoal (10% Pd). 0.25 g of (2R,4R)-3-[3-{2-[4-tert-butoxycarbonyl...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
C1CSC[NH]1.c1ccccc1.c1ccccc1.c1ccccc1
Other
[Pd]
null
null
CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)OCc2ccccc2)c1>[Pd]>CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CNC(=O)Nc1cccc(CC(=O)O)c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-acb9658cde0548e0a200ac19f404869d
CC(C)(C)OC(=O)C(N)C(=O)N1[C@@H](c2ccccc2-c2ccccc2)SC[C@H]1C(=O)OC(C)(C)C.CC(C)(C)OC(=O)NCC(=O)O>>CC(C)(C)OC(=O)NCC(=O)N1[C@@H](c2ccccc2-c2ccccc2)SC[C@H]1C(=O)OC(C)(C)C
C1(CCCCC1)N=C=NC1CCCCC1.C(C)(C)(C)OC(=O)C(C(=O)N1[C@H](SC[C@H]1C(=O)OC(C)(C)C)C1=C(C=CC=C1)C1=CC=CC=C1)N.C1(=CC=CC=C1)C1=C(C=CC=C1)C1SC[C@H](N1)C(=O)OC(C)(C)C.C(C)(C)(C)OC(=O)NCC(=O)O>>C(C)(C)(C)OC(=O)NCC(=O)N1[C@H](SC[C@H]1C(=O)OC(C)(C)C)C1=C(C=CC=C1)C1=CC=CC=C1
CC(C)(C)OC(=O)[CH:9]([NH2:8])[C:10](=[O:11])[N:12]1[C@@H:13]([c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]2-[c:20]2[cH:21][cH:22][cH:23][cH:24][cH:25]2)[S:26][CH2:27][C@H:28]1[C:29](=[O:30])[O:31][C:32]([CH3:33])([CH3:34])[CH3:35].O=C(O)CN[C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5]...
CC(C)(C)OC(=O)C(N)C(=O)N1[C@@H](c2ccccc2-c2ccccc2)SC[C@H]1C(=O)OC(C)(C)C.CC(C)(C)OC(=O)NCC(=O)O
CC(C)(C)OC(=O)NCC(=O)N1[C@@H](c2ccccc2-c2ccccc2)SC[C@H]1C(=O)OC(C)(C)C
null
null
null
Protection
OtherReaction
35d42f1e7ecc8f0be03450644bb70a362f1e1038fcc33f290b2cccc629937aca
fd660e5850eedebb186615721848051bbc41c15a8337b192fa3ead00371112ac
c1ccc(-c2ccccc2[C@@H]2NCCS2)cc1
C-C(-C)(-C)-O-C(=O)-[CH;D3;+0:1](-[NH2;D1;+0:2])-[C:3](=[O;D1;H0:4])-[#7:5](-[C:6]-[#16:7])-[C:8]-[C:9](-[#8:10])=[O;D1;H0:11].O-C(=O)-C-N-[C;H0;D3;+0:12](=[O;D1;H0:13])-[#8:14]-[C:15](-[C;D1;H3:16])(-[C;D1;H3:17])-[C;D1;H3:18]>>[#16:7]-[C:6]-[#7:5](-[C:3](=[O;D1;H0:4])-[CH2;D2;+0:1]-[NH;D2;+0:2]-[C;H0;D3;+0:12](=[O;D1...
null
[]
null
null
null
null
C tert-Butyl (2R,4R)-3-(2-tert-butoxycarbonyl-aminoacetyl)-2-(2-phenylphenyl)-4-thiazolidinecarboxylate may be prepared in a manner similar to that described in Example 1C, but starting with 5.44 g of tert-butyl (2RS,4R)-2-(2-phenylphenyl)-4-thiazolidinecarboxylate, 2.8 g of 2-tert-butoxycarbonylaminoacetic acid and 3....
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Carboxylic acid.Ester.Ether.Primary amine.Boc.Boc
Carbamic ester.Ether.Boc
null
null
C1CSC[NH]1.c1ccccc1.c1ccccc1
HO-
null
null
null
CC(C)(C)OC(=O)C(N)C(=O)N1[C@@H](c2ccccc2-c2ccccc2)SC[C@H]1C(=O)OC(C)(C)C.CC(C)(C)OC(=O)NCC(=O)O>>CC(C)(C)OC(=O)NCC(=O)N1[C@@H](c2ccccc2-c2ccccc2)SC[C@H]1C(=O)OC(C)(C)C
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-e580b3e86a874597a7a65767dd4dd35e
CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CN.Cc1cccc(N=C=O)c1>>Cc1cccc(NC(=O)NCC(=O)N2[C@@H](c3ccccc3-c3ccccc3)SC[C@H]2C(=O)OC(C)(C)C)c1
NCC(=O)N1[C@H](SC[C@H]1C(=O)OC(C)(C)C)C1=C(C=CC=C1)C1=CC=CC=C1.CC=1C=C(C=CC1)N=C=O>>CC=1C=C(C=CC1)NC(NCC(=O)N1[C@H](SC[C@H]1C(=O)OC(C)(C)C)C1=C(C=CC=C1)C1=CC=CC=C1)=O
[NH2:10][CH2:11][C:12](=[O:13])[N:14]1[C@@H:15]([c:16]2[cH:17][cH:18][cH:19][cH:20][c:21]2-[c:22]2[cH:23][cH:24][cH:25][cH:26][cH:27]2)[S:28][CH2:29][C@H:30]1[C:31](=[O:32])[O:33][C:34]([CH3:35])([CH3:36])[CH3:37].[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]([N:7]=[C:8]=[O:9])[cH:38]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]([NH:...
CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CN.Cc1cccc(N=C=O)c1
Cc1cccc(NC(=O)NCC(=O)N2[C@@H](c3ccccc3-c3ccccc3)SC[C@H]2C(=O)OC(C)(C)C)c1
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCC(=O)N1CCS[C@@H]1c1ccccc1-c1ccccc1)Nc1ccccc1
[#16:1]-[C:2]-[#7:3](-[C:4](=[O;D1;H0:5])-[C:6]-[NH2;D1;+0:7])-[C:8]-[C:9](-[#8:10])=[O;D1;H0:11].[O;D1;H0:12]=[C;H0;D2;+0:13]=[N;H0;D2;+0:14]-[c:15](:[c:16]):[c:17]>>[#16:1]-[C:2]-[#7:3](-[C:4](=[O;D1;H0:5])-[C:6]-[NH;D2;+0:7]-[C;H0;D3;+0:13](=[O;D1;H0:12])-[NH;D2;+0:14]-[c:15](:[c:16]):[c:17])-[C:8]-[C:9](-[#8:10])=[...
12.5
[{"value": 12.5, "product": "CC=1C=C(C=CC1)NC(NCC(=O)N1[C@H](SC[C@H]1C(=O)OC(C)(C)C)C1=C(C=CC=C1)C1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The procedure is similar to that described in Example 1A, but starting with 1.32 g of tert-butyl (2R,4R)-3-(2-aminoacetyl)-2-(2-phenylphenyl)-4-thiazolidinecarboxylate and 0.47 g of 3-methylphenyl isocyanate. The crude product is purified by chromatography on silica [eluent: methylene chloride/ethyl acetate (90:10 by v...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccccc1.c1ccccc1.C1CSC[NH]1
null
null
null
null
CC(C)(C)OC(=O)[C@@H]1CS[C@H](c2ccccc2-c2ccccc2)N1C(=O)CN.Cc1cccc(N=C=O)c1>>Cc1cccc(NC(=O)NCC(=O)N2[C@@H](c3ccccc3-c3ccccc3)SC[C@H]2C(=O)OC(C)(C)C)c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-5ea1469a8e4446d8bece6f8a474dd542
CON=C(C(=O)OC)c1ccccc1/C=C(\Cl)C(=O)OC(C)(C)C>>CON=C(C(=O)OC)c1ccccc1/C=C(\Cl)C(=O)O
CON=C(C(=O)OC)C1=C(C=CC=C1)\C=C(\C(=O)OC(C)(C)C)/Cl.C([O-])([O-])=O.[Na+].[Na+].C(C)(C)(C)OC>>CON=C(C(=O)OC)C1=C(C=CC=C1)\C=C(\C(=O)O)/Cl
CC(C)(C)[O:20][C:18](/[C:16](=[CH:15]/[c:14]1[c:9]([C:4](=[N:3][O:2][CH3:1])[C:5](=[O:6])[O:7][CH3:8])[cH:10][cH:11][cH:12][cH:13]1)[Cl:17])=[O:19]>>[CH3:1][O:2][N:3]=[C:4]([C:5](=[O:6])[O:7][CH3:8])[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1/[CH:15]=[C:16](\[Cl:17])[C:18](=[O:19])[OH:20]
CON=C(C(=O)OC)c1ccccc1/C=C(\Cl)C(=O)OC(C)(C)C
CON=C(C(=O)OC)c1ccccc1/C=C(\Cl)C(=O)O
null
null
ClCCl.FC(C(=O)O)(F)F
Deprotection
Deprotection of carboxylic acid
152e5537e48c95b4a3e767536b0f9f68d1308e5f484070828ab5ed951805157a
7f019d4cfe9b3036d0a2d3a3209aa0e1fcb05418ebee15a4be5e125d315d5f01
c1ccccc1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])/[C:4](-[Cl;D1;H0:5])=[C:6]/[c:7]>>[Cl;D1;H0:5]/[C:4](=[C:6]\[c:7])-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
82
[{"value": 82.0, "product": "CON=C(C(=O)OC)C1=C(C=CC=C1)\\C=C(\\C(=O)O)/Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
29 g of methyl 2-methoxyimino-2-{2-[2-chloro-2-tert-butyloxycarbonyl-(Z)-ethenyl]phenyl}acetate from Example 3 are stirred in a mixture of 40 ml of trifluoroacetic acid and 160 ml of dichloromethane for 2.5 hours at room temperature. The dark solution is then stirred into 500 ml of saturated sodium carbonate solution (...
10.6084/m9.figshare.5104873.v1
null
Ester.Boc
Carboxylic acid
null
null
c1ccccc1
Other
ClCCl.FC(C(=O)O)(F)F
null
null
CON=C(C(=O)OC)c1ccccc1/C=C(\Cl)C(=O)OC(C)(C)C>ClCCl.FC(C(=O)O)(F)F>CON=C(C(=O)OC)c1ccccc1/C=C(\Cl)C(=O)O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d3d3361c405f4232a9008dac1542cd34
COC(=O)CN=[N+]=[N-].O=Cc1ccc2c(c1)CCO2>>COC(=O)C(=Cc1ccc2c(c1)CCO2)N=[N+]=[N-]
CC(C)([O-])C.[K+].O1CCC2=C1C=CC(=C2)C=O.N(=[N+]=[N-])CC(=O)OC>>COC(C(=CC=1C=CC2=C(CCO2)C1)N=[N+]=[N-])=O
[CH3:1][O:2][C:3](=[O:4])[CH2:5][N:16]=[N+:17]=[N-:18].O=[CH:6][c:7]1[cH:8][cH:9][c:10]2[c:11]([cH:12]1)[CH2:13][CH2:14][O:15]2>>[CH3:1][O:2][C:3](=[O:4])[C:5](=[CH:6][c:7]1[cH:8][cH:9][c:10]2[c:11]([cH:12]1)[CH2:13][CH2:14][O:15]2)[N:16]=[N+:17]=[N-:18]
COC(=O)CN=[N+]=[N-].O=Cc1ccc2c(c1)CCO2
COC(=O)C(=Cc1ccc2c(c1)CCO2)N=[N+]=[N-]
null
null
CO
C-C Coupling
Aldol condensation
a86984aeb4a9963534e0b081b0ecca18455fda1775f36ce168d1ca4cf966df3e
203dd34a20dceaf1737adbf20e01b43c2424e4e4b1722d942d1a796d895396e6
c1ccc2c(c1)CCO2
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]
94.2
[{"value": 94.2, "product": "COC(C(=CC=1C=CC2=C(CCO2)C1)N=[N+]=[N-])=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-10
CELSIUS
1
HOUR
To a cold (-10° C.) stirred solution of potassium tert-butoxide (6.06 g) in dry methanol (40 ml) was added dropwise a mixture of 2,3-dihydrobenzofuran-5-carboxaldehyde (2 g) and methyl azidoacetate (6.21 g). The mixture was stirred for 1 h at -10° C. and then stored at 0° C. for 18 h. The resulting pale yellow microcry...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester
Ester
null
null
c1ccc2c(c1)CCO2
HO-
CO
-10
1
COC(=O)CN=[N+]=[N-].O=Cc1ccc2c(c1)CCO2>CO>COC(=O)C(=Cc1ccc2c(c1)CCO2)N=[N+]=[N-]
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-327e2608ec0144c2b599ca59201375d2
CCOC(CBr)OCC.Nc1cccc2c1CCCO2>>CCOC(CNc1cccc2c1CCCO2)OCC
C(C)OC(CBr)OCC.O1CCCC2=C(C=CC=C12)N.C([O-])([O-])=O.[K+].[K+]>>O1CCCC2=C(C=CC=C12)NCC(OCC)OCC
Br[CH2:5][CH:4]([O:3][CH2:2][CH3:1])[O:17][CH2:18][CH3:19].[NH2:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]1[CH2:13][CH2:14][CH2:15][O:16]2>>[CH3:1][CH2:2][O:3][CH:4]([CH2:5][NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]1[CH2:13][CH2:14][CH2:15][O:16]2)[O:17][CH2:18][CH3:19]
CCOC(CBr)OCC.Nc1cccc2c1CCCO2
CCOC(CNc1cccc2c1CCCO2)OCC
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
fc19a1445ff204e66e51735d0191465bda3c6691fd233624a54742c9d4828411
0b1d32f56ad00f1e5bdae9390f9227bbea012fa2f8203aac34726b8a6761cc7c
c1ccc2c(c1)CCCO2
Br-[CH2;D2;+0:1]-[C:2](-[#8:3])-[#8:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[#8:3]-[C:2](-[#8:4])-[CH2;D2;+0:1]-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]
null
[]
100
CELSIUS
null
null
Bromoacetaldehyde diethyl acetal (11.8 ml) was added to a mixture of chroman-5-yl-amine (5.85 g) (prepared according to J. Heterocyclic Chem., (1973), Vol 10 (4) page 623), and potassium carbonate (10.84 g) in dry DMF (70 ml) at room temperature under N2. The mixture was heated at 100° C. for 60 h. The cooled mixture w...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary amine
Secondary amine
null
null
c1ccc2c(c1)CCCO2
HBr
CN(C)C=O
100
null
CCOC(CBr)OCC.Nc1cccc2c1CCCO2>CN(C)C=O>CCOC(CNc1cccc2c1CCCO2)OCC
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-83e005a4175642fe9afc52764d88855b
CCOC(CBr)OCC.Nc1cccc2c1CCO2>>CCOC(CNc1cccc2c1CCO2)OCC
O1CCC2=C1C=CC=C2N.C([O-])([O-])=O.[K+].[K+].C(C)OC(CBr)OCC>>C(C)OC(CNC1=CC=CC2=C1CCO2)OCC
Br[CH2:5][CH:4]([O:3][CH2:2][CH3:1])[O:16][CH2:17][CH3:18].[NH2:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]1[CH2:13][CH2:14][O:15]2>>[CH3:1][CH2:2][O:3][CH:4]([CH2:5][NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]1[CH2:13][CH2:14][O:15]2)[O:16][CH2:17][CH3:18]
CCOC(CBr)OCC.Nc1cccc2c1CCO2
CCOC(CNc1cccc2c1CCO2)OCC
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
fc19a1445ff204e66e51735d0191465bda3c6691fd233624a54742c9d4828411
0b1d32f56ad00f1e5bdae9390f9227bbea012fa2f8203aac34726b8a6761cc7c
c1ccc2c(c1)CCO2
Br-[CH2;D2;+0:1]-[C:2](-[#8:3])-[#8:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[#8:3]-[C:2](-[#8:4])-[CH2;D2;+0:1]-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]
null
[]
100
CELSIUS
null
null
A mixture of 2,3-dihydro-benzofuran-4-ylamine (preparation. J. Hetereocyclic Chem., 18, 1333 (1980)) (4.34 g), potassium carbonate (8.87 g) and bromo acetaldehyde diethyl acetal (9.7 ml) in dry DMF (60 ml) was heated to 100° C. for 2 days under. The mixture was cooled and was partitioned between water and ethyl acetate...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary amine
Secondary amine
null
null
c1ccc2c(c1)CCO2
HBr
CN(C)C=O
100
null
CCOC(CBr)OCC.Nc1cccc2c1CCO2>CN(C)C=O>CCOC(CNc1cccc2c1CCO2)OCC
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-369807e9e22041ffb2a801a6f750a115
CC(=O)OC(C)=O.c1cc2ccc3c(c2[nH]1)CCO3>>CC(=O)NCCN1CCc2ccc3c(c21)CCO3
C(C)(=O)OC(C)=O.N1C=CC2=CC=C3C(=C12)CCO3.N1=CC=CC=C1>>N1(CCC2=CC=C3C(=C12)CCO3)CCNC(C)=O
CC(=O)O[C:2]([CH3:1])=[O:3].[cH:6]1[nH:7][c:15]2[c:10]([cH:9]1)[cH:11][cH:12][c:13]1[c:14]2[CH2:16][CH2:17][O:18]1>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][c:10]2[cH:11][cH:12][c:13]3[c:14]([c:15]21)[CH2:16][CH2:17][O:18]3
CC(=O)OC(C)=O.c1cc2ccc3c(c2[nH]1)CCO3
CC(=O)NCCN1CCc2ccc3c(c21)CCO3
null
null
C1CCOC1
Acylation
OtherReaction
43dbdc8998fd15afdab1b5d3332fcf7dcf4e1cd3bef06be9df6ebe43daa7c853
a1f7403337b0cb17f86436f8a329ecbaeddd4f0fb6dc049f1812ab8355b89185
c1cc2c(c3c1CCN3)CCO2
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[c:4]:[c:5]1:[cH;D2;+0:6]:[cH;D2;+0:7]:[nH;D2;+0:8]:[c:9]:1:[c:10]>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[#7:11]-[C:12]-[CH2;D2;+0:7]-[N;H0;D3;+0:8]1-[C:13]-[CH2;D2;+0:6]-[c:5](:[c:4]):[c:9]-1:[c:10]
null
[]
null
null
null
null
To a stirred solution of Intermediate 7 (77 mg) in dry THF (5 ml) containing pyridine (0.09 ml) was added acetic anhydride (0.06 ml). After 18 h at 20° C. the mixture was partitioned between 2N Na2CO3 (30 ml) and EtOAc (2×30 ml). The dried extracts were evaporated and the residue chromatographed on silica gel (20 g). E...
10.6084/m9.figshare.5104873.v1
null
Anhydride
Secondary amide.Tertiary amine
c1cc2ccc3c(c2[nH]1)CCO3
c1cc2c(c3c1CC[NH]3)CCO2
c1cc2c(c3c1CC[NH]3)CCO2
Other
C1CCOC1
null
null
CC(=O)OC(C)=O.c1cc2ccc3c(c2[nH]1)CCO3>C1CCOC1>CC(=O)NCCN1CCc2ccc3c(c21)CCO3
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-6f742d84ff9d4b8e8717082162d207dc
Cl>>Cl
N1(CCC2=CC=C3C(=C12)CCO3)CCNC(C)=O.Cl>>Cl.N1(CCC2=CC=C3C(=C12)CCO3)CCNC(C)=O
[ClH:19]>>[ClH:19]
Cl
Cl
null
null
C(C)(=O)OCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
null
null
2
HOUR
The title compound of Example 3 (334 mg) was dissolved in ethyl acetate (20 ml) and was treated with ethereal HCl (1.35 ml). This was stirred at room temperature for 2 h and then the solvent was evaporated to give the title compound as a pale green powder (383 mg), m.p. 152°-154° C. Conditions: See reaction.notes.proce...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
C(C)(=O)OCC
null
2
Cl>C(C)(=O)OCC>Cl
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-dd274f47e9044758accf665671201e6c
CC(=O)NCCCl.CC(C)=O.Nc1cccc2c1CCCO2>>CC(=O)NCCN1CCc2ccc3c(c21)CCO3
O1CCCC2=C(C=CC=C12)N.[I-].[K+].ClCCNC(C)=O.CC(=O)C>>N1(CCC2=CC=C3C(=C12)CCO3)CCNC(C)=O
Cl[CH2:6][CH2:5][NH:4][C:2]([CH3:1])=[O:3].CC(=O)[CH3:8].[NH2:7][c:15]1[cH:10][cH:11][cH:12][c:13]2[c:14]1[CH2:9][CH2:16][CH2:17][O:18]2>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][c:10]2[cH:11][cH:12][c:13]3[c:14]([c:15]21)[CH2:16][CH2:17][O:18]3
CC(=O)NCCCl.CC(C)=O.Nc1cccc2c1CCCO2
CC(=O)NCCN1CCc2ccc3c(c21)CCO3
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
95ab9d697bba91fc1ac3efad48a78c7aefd69c2f6b85a7733edd521a24d73e6b
fedc0382ba58f6b119b2623cb03d1ba36f77720ea27e54609811232a45a383e6
c1cc2c(c3c1CCN3)CCO2
C-C(=O)-[CH3;D1;+0:1].Cl-[CH2;D2;+0:2]-[C:3]-[#7:4]-[C:5](-[C;D1;H3:6])=[O;D1;H0:7].[NH2;D1;+0:8]-[c:9]1:[cH;D2;+0:10]:[c:11]:[c:12]:[c:13]2:[c;H0;D3;+0:14]:1-[CH2;D2;+0:15]-[CH2;D2;+0:16]-[C:17]-[#8:18]-2>>[C;D1;H3:6]-[C:5](=[O;D1;H0:7])-[#7:4]-[C:3]-[CH2;D2;+0:2]-[N;H0;D3;+0:8]1-[CH2;D2;+0:1]-[CH2;D2;+0:15]-[c;H0;D3;...
null
[]
null
null
null
null
A mixture of Intermediate 4 (50 mg), potassium iodide (1 g) and N-(2-chloroethyl)acetamide (96 mg) in acetone (5 ml) was heated to reflux for 2 days. The cooled mixture was partitioned between water and ethyl acetate. The extracts were dried, and evaporated, and the residue chromatographed on silica gel. Elution with C...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Primary amine
Tertiary amine
c1ccc2c(c1)CCCO2
c1cc2c(c3c1CC[NH]3)CCO2
c1cc2c(c3c1CC[NH]3)CCO2
HCl
null
null
null
CC(=O)NCCCl.CC(C)=O.Nc1cccc2c1CCCO2>>CC(=O)NCCN1CCc2ccc3c(c21)CCO3
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-cd36f8dd6fc646be8d7824e16eaca0f5
CCCN(CCC)C1CC2CN(C(=O)c3ccccc3)C3=C2C(C1)C(Br)C=C3>>CCCN(CCC)C1Cc2c(C#N)ccc3c2C(C1)CN3C(=O)c1ccccc1
C(C1=CC=CC=C1)(=O)N1CC2C=3C(C(C=CC13)Br)CC(C2)N(CCC)CCC.C(#N)[Cu]>>C(C1=CC=CC=C1)(=O)N1CC2C=3C(=C(C=CC13)C#N)CC(C2)N(CCC)CCC
Br[CH:11]1[CH:14]=[CH:15][C:16]2=[C:17]3[CH:10]([CH2:9][CH:8]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH2:6][CH3:7])[CH2:19][CH:18]13)[CH2:20][N:21]2[C:22](=[O:23])[c:24]1[cH:25][cH:26][cH:27][cH:28][cH:29]1>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7])[CH:8]1[CH2:9][c:10]2[c:11]([C:12]#[N:13])[cH:14][cH:15][c:16]3[c:...
CCCN(CCC)C1CC2CN(C(=O)c3ccccc3)C3=C2C(C1)C(Br)C=C3
CCCN(CCC)C1Cc2c(C#N)ccc3c2C(C1)CN3C(=O)c1ccccc1
null
[Cu]I
O.CN(C)C=O.C(Cl)Cl
Aromatic Heterocycle Formation
OtherReaction
b1b7d399944a8d47a218d4a804f2d01edbc5dfec2a79dc868f640aafe591af24
13bad28d5b0a0a6678ff3c47616bbe6f1ca115a480d3e72288190f082dcfe4ee
O=C(c1ccccc1)N1CC2CCCc3cccc1c32
Br-[CH;D3;+0:1]1-[CH;D2;+0:2]=[CH;D2;+0:3]-[C;H0;D3;+0:4]2=[C;H0;D3;+0:5]3-[CH;D3;+0:6](-[C:7]-[C:8]-[C:9]-[CH;D3;+0:10]-3-1)-[CH2;D2;+0:11]-[#7:12]-2-[C:13](=[O;D1;H0:14])-[c:15]>>[N;D1;H0:16]#[C:17]-[c;H0;D3;+0:1]1:[cH;D2;+0:2]:[cH;D2;+0:3]:[c;H0;D3;+0:4]2:[c;H0;D3;+0:5]3:[c;H0;D3;+0:6]:1-[C:7]-[C:8]-[C:9]-[CH;D3;+0:...
82.6
[{"value": 82.6, "product": "C(C1=CC=CC=C1)(=O)N1CC2C=3C(=C(C=CC13)C#N)CC(C2)N(CCC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
140
CELSIUS
6
HOUR
To a solution of (±)-1-benzoyl-6-bromo-4-(di-n-propylamino)hexahydrobenz[cd]indole (5.5 g, 12.5 mmol) in DMF (100 mL) under a N2 atmosphere was added 3.4 g (37.5 mmol) of CuCN and 7.1 g (37.5 mmol) of CuI. The reaction mixture was then stirred at 140° C. for 6 hr. The reaction mixture was poured onto ice, diluted with ...
10.6084/m9.figshare.5104873.v1
null
Enamine.Secondary halide
Nitrile
C1=CC2=C3C(C1)CCCC3C[NH]2
c1cc2c3c(c1)[NH]CC3CCC2
c1cc2c3c(c1)[NH]CC3CCC2.c1ccccc1
HBr
[Cu]I.O.CN(C)C=O.C(Cl)Cl
140
6
CCCN(CCC)C1CC2CN(C(=O)c3ccccc3)C3=C2C(C1)C(Br)C=C3>[Cu]I.O.CN(C)C=O.C(Cl)Cl>CCCN(CCC)C1Cc2c(C#N)ccc3c2C(C1)CN3C(=O)c1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-90bc15899b3542d1bd25e6cafd9e8880
CCCN(CCC)C1Cc2c(C#N)ccc3c2C(C1)CN3C(=O)c1ccccc1>>CCCN(CCC)C1Cc2c(C#N)ccc3c2C(CN3)C1
Cl.C(CCC)[Li].C(C1=CC=CC=C1)(=O)N1CC2C=3C(=C(C=CC13)C#N)CC(C2)N(CCC)CCC>>C(#N)C1=C2C=3C(CNC3C=C1)CC(C2)N(CCC)CCC
O=C(c1ccccc1)[N:20]1[c:16]2[cH:15][cH:14][c:11]([C:12]#[N:13])[c:10]3[c:17]2[CH:18]([CH2:19]1)[CH2:21][CH:8]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH2:6][CH3:7])[CH2:9]3>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7])[CH:8]1[CH2:9][c:10]2[c:11]([C:12]#[N:13])[cH:14][cH:15][c:16]3[c:17]2[CH:18]([CH2:19][NH:20]3)[CH2:21...
CCCN(CCC)C1Cc2c(C#N)ccc3c2C(C1)CN3C(=O)c1ccccc1
CCCN(CCC)C1Cc2c(C#N)ccc3c2C(CN3)C1
null
null
CCCCCC.C1CCOC1
Reduction
Hydrogenolysis of tertiary amines
99f0a6dc5611581d1d7a71900cee1ca5de3aaa1efd3b5fccc3b6d24420f211d3
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
c1cc2c3c(c1)NCC3CCC2
O=C(-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[c:4]:[c:5]-1:[c:6])-c1:c:c:c:c:c:1>>[c:6]:[c:5]1:[c:4]-[C:3]-[C:2]-[NH;D2;+0:1]-1
113.8
[{"value": 113.8, "product": "C(#N)C1=C2C=3C(CNC3C=C1)CC(C2)N(CCC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
30
MINUTE
To a stirred solution of 4.8 g (0.0124 mol) of (±)-1-benzoyl-6-cyano-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole in 200 mL of THF cooled to -78° C. under a N2 atmosphere were added 16 mL (0.025 mol) of a 1.6M solution of n-butyl lithium in hexane. The reaction mixture was stirred at -78° C. for 30 minutes...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccccc1.c1cc2c3c(c1)[NH]CC3CCC2
c1cc2c3c(c1)NCC3CCC2
c1cc2c3c(c1)NCC3CCC2
HO-
CCCCCC.C1CCOC1
-78
0.5
CCCN(CCC)C1Cc2c(C#N)ccc3c2C(C1)CN3C(=O)c1ccccc1>CCCCCC.C1CCOC1>CCCN(CCC)C1Cc2c(C#N)ccc3c2C(CN3)C1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-4da5a68747f9476cb34b56f4b3dcbceb
CCCN(CCC)C1Cc2c(C#N)ccc3c2C(CN3)C1>>CCCN(CCC)C1Cc2c(C(C)=O)ccc3c2C(CN3)C1
C(#N)C1=C2C=3C(CNC3C=C1)CC(C2)N(CCC)CCC.C[Mg]Br.C(C)OCC.[NH4+].[Cl-]>>C(C)(=O)C1=C2C=3C(CNC3C=C1)CC(C2)N(CCC)CCC
N#[C:12][c:11]1[c:10]2[c:18]3[c:17]([cH:16][cH:15]1)[NH:21][CH2:20][CH:19]3[CH2:22][CH:8]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH2:6][CH3:7])[CH2:9]2>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7])[CH:8]1[CH2:9][c:10]2[c:11]([C:12]([CH3:13])=[O:14])[cH:15][cH:16][c:17]3[c:18]2[CH:19]([CH2:20][NH:21]3)[CH2:22]1
CCCN(CCC)C1Cc2c(C#N)ccc3c2C(CN3)C1
CCCN(CCC)C1Cc2c(C(C)=O)ccc3c2C(CN3)C1
null
null
C1=CC=CC=C1
Miscellaneous
OtherReaction
54622de249eb9a5622e28710a02d261b08e09c3ee957106ef84a0e4751ccb30f
957d5e0aaa82a4f5b73d699040cb2acd7f615417c9e400cbb7a63fa4c133449a
c1cc2c3c(c1)NCC3CCC2
N#[C;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[C;D1;H3:5]-[C;H0;D3;+0:1](=[O;D1;H0:6])-[c:2](:[c:3]):[c:4]
null
[]
null
null
30
MINUTE
A solution of 0.5 g (1.8 mmol) of (±)-6-cyano-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole in 75 mL of benzene was treated with 5 mL of 2.0M methylmagnesium bromide in diethyl ether. The reaction mixture was refluxed for 2 days. The reaction mixture was cooled and excess Grignard reagent was decomposed wit...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Ketone
null
null
c1cc2c3c(c1)NCC3CCC2
null
C1=CC=CC=C1
null
0.5
CCCN(CCC)C1Cc2c(C#N)ccc3c2C(CN3)C1>C1=CC=CC=C1>CCCN(CCC)C1Cc2c(C(C)=O)ccc3c2C(CN3)C1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-4c6265efbbae45d2a4a86f843d116b35
CCCN(CCC)C1Cc2c(C(C)=O)ccc3c2C(CN3)C1.O=C(Cl)OCC(Cl)(Cl)Cl>>NC(=O)N1CCc2ccccc21
C(C)(=O)C1=C2C=3C(CNC3C=C1)CC(C2)N(CCC)CCC.C(C)N(CC)CC.ClC(=O)OCC(Cl)(Cl)Cl>>C(N)(=O)N1CCC2=CC=CC=C12
CCCN(CCC)C1C[CH:6]2[CH2:5][NH:4][c:12]3[c:7]2[c:8]([c:9](C(C)=O)[cH:10][cH:11]3)C1.ClC(Cl)(Cl)CO[C:2](Cl)=[O:3]>>[NH2:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]21
CCCN(CCC)C1Cc2c(C(C)=O)ccc3c2C(CN3)C1.O=C(Cl)OCC(Cl)(Cl)Cl
NC(=O)N1CCc2ccccc21
null
null
C(Cl)Cl
Acylation
OtherReaction
6a9ab0c72d3ef4f5776b87b216245ab6ebe0245f6ae66f5b216d5863946ee678
1fea30f316824198e233dc7d7d5f0ed1a4a322c4c89c24d4336ce38c6250dbb8
c1ccc2c(c1)CCN2
C-C-C-N(-C-C-C)-C1-C-[CH;D3;+0:1]2-[C:2]-[NH;D2;+0:3]-[c:4]3:[c:5]:[c:6]:[c;H0;D3;+0:7](-C(-C)=O):[c;H0;D3;+0:8](:[c:9]:3-2)-C-1.Cl-[C;H0;D3;+0:10](=[O;D1;H0:11])-O-C-C(-Cl)(-Cl)-Cl>>[N;D1;H2:12]-[C;H0;D3;+0:10](=[O;D1;H0:11])-[N;H0;D3;+0:3]1-[C:2]-[CH2;D2;+0:1]-[c:9]2:[cH;D2;+0:8]:[cH;D2;+0:7]:[c:6]:[c:5]:[c:4]:2-1
null
[]
null
null
1
HOUR
To a solution of (±)-6-acetyl-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole (2.3 g, 7.7 mmol) and triethylamine (1.1 ml, 8 mmol) in 90 ml CH2Cl2 under N2 was added dropwise a solution of 2,2,2-trichloroethyl chloroformate. The reaction mixture was stirred at room temperature for 1 hr. The CH2Cl2 solution wa...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Trichloro group.Ketone.Ether.Secondary amine.Tertiary amine
Urea
c1cc2c3c(c1)NCC3CCC2
c1ccc2c(c1)CC[NH]2
c1ccc2c(c1)CC[NH]2
HCl
C(Cl)Cl
null
1
CCCN(CCC)C1Cc2c(C(C)=O)ccc3c2C(CN3)C1.O=C(Cl)OCC(Cl)(Cl)Cl>C(Cl)Cl>NC(=O)N1CCc2ccccc21
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a9838402e244479d887e1b79c36d8441
CCCN(CCC)[C@H]1Cc2c(C(C)=O)ccc3c2[C@@H](CN3)C1.O=C(Cl)OCC(Cl)(Cl)Cl>>NC(=O)N1CCc2ccccc21
C(C)(=O)C1=C2C=3[C@@H](CNC3C=C1)C[C@H](C2)N(CCC)CCC.C(C)N(CC)CC.ClC(=O)OCC(Cl)(Cl)Cl>>C(N)(=O)N1CCC2=CC=CC=C12
CCCN(CCC)[C@@H]1C[C@@H:6]2[CH2:5][NH:4][c:12]3[c:7]2[c:8]([c:9](C(C)=O)[cH:10][cH:11]3)C1.ClC(Cl)(Cl)CO[C:2](Cl)=[O:3]>>[NH2:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]21
CCCN(CCC)[C@H]1Cc2c(C(C)=O)ccc3c2[C@@H](CN3)C1.O=C(Cl)OCC(Cl)(Cl)Cl
NC(=O)N1CCc2ccccc21
null
null
C(Cl)Cl
Acylation
OtherReaction
225a7c62dff362372b072d49673129934807b8d7bc79257f934cb235926ab1cb
1fea30f316824198e233dc7d7d5f0ed1a4a322c4c89c24d4336ce38c6250dbb8
c1ccc2c(c1)CCN2
null
270.4
[{"value": 270.4, "product": "C(N)(=O)N1CCC2=CC=CC=C12", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of (+)(2aS,4R)-6-acetyl-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole (1.7 g, 5.7 mmol) and triethylamine (0.8 ml, 6 mmol) in 90 ml CH2Cl2 was added dropwise a solution of 2,2,2-trichloroethyl chloroformate (1.3 g, 6 mmol) in 10 ml CH2Cl2. The reaction mixture was stirred at room temperature f...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Trichloro group.Ketone.Ether.Secondary amine.Tertiary amine
Urea
c1cc2c3c(c1)NC[C@H]3CCC2
c1ccc2c(c1)CC[NH]2
c1ccc2c(c1)CC[NH]2
HCl
C(Cl)Cl
null
1
CCCN(CCC)[C@H]1Cc2c(C(C)=O)ccc3c2[C@@H](CN3)C1.O=C(Cl)OCC(Cl)(Cl)Cl>C(Cl)Cl>NC(=O)N1CCc2ccccc21
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-06c509707e6944338237e366af75ab71
CCCN(CCC)[C@@H]1Cc2c(I)ccc3c2[C@@H](C1)CN3C(=O)c1ccccc1.CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ncco1>>CCCN(CCC)[C@@H]1Cc2c(-c3ncco3)ccc3c2[C@@H](C1)CN3C(=O)c1ccccc1
C(CCC)[Sn](C=1OC=CN1)(CCCC)CCCC.C(C1=CC=CC=C1)(=O)N1C[C@H]2C=3C(=C(C=CC13)I)C[C@H](C2)N(CCC)CCC>>C(C1=CC=CC=C1)(=O)N1C[C@H]2C=3C(=C(C=CC13)C=1OC=CN1)C[C@H](C2)N(CCC)CCC
I[c:11]1[c:10]2[c:20]3[c:19]([cH:18][cH:17]1)[N:24]([C:25](=[O:26])[c:27]1[cH:28][cH:29][cH:30][cH:31][cH:32]1)[CH2:23][C@@H:21]3[CH2:22][C@H:8]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH2:6][CH3:7])[CH2:9]2.CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c:12]1[n:13][cH:14][cH:15][o:16]1>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7]...
CCCN(CCC)[C@@H]1Cc2c(I)ccc3c2[C@@H](C1)CN3C(=O)c1ccccc1.CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ncco1
CCCN(CCC)[C@@H]1Cc2c(-c3ncco3)ccc3c2[C@@H](C1)CN3C(=O)c1ccccc1
null
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1
C1(=CC=CC=C1)C
C-C Coupling
Stille reaction_aryl
42596528f1dffb674d4997eac8515a130029c7feafaf2f052b8fa314683b7946
db27eeefac0475c6d74fa10b3167e95a61caaae74e8bbafd45892452c0c3d4d6
O=C(c1ccccc1)N1C[C@@H]2CCCc3c(-c4ncco4)ccc1c32
C-C-C-[CH2]-[Sn](-[CH2]-C-C-C)(-[CH2]-C-C-C)-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#8;a:5]:1.I-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](:[c:10])-[C:11]>>[C:11]-[c:9](:[c:10]):[c;H0;D3;+0:6](-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#8;a:5]:1):[c:7]:[c:8]
67.5
[{"value": 67.5, "product": "C(C1=CC=CC=C1)(=O)N1C[C@H]2C=3C(=C(C=CC13)C=1OC=CN1)C[C@H](C2)N(CCC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 5.0 g (13.8 mmol) of the crude 2-tributylstannyloxazole prepared above and 6.8 g (13.9 mmol) of (+)(2aR,4S)-1-benzoyl-6-iodo-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole in 100 ml of toluene was treated with 0.7 g (0.6 mmol) of tetrakis(triphenylphosphine)palladium then refluxed under nitroge...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tin
null
c1cc2c3c(c1)[NH]C[C@@H]3CCC2.c1cocn1
c1cocn1.c1cc2c3c(c1)[NH]C[C@@H]3CCC2
c1cocn1.c1cc2c3c(c1)[NH]C[C@@H]3CCC2.c1ccccc1
HI.Sn
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.C1(=CC=CC=C1)C
null
null
CCCN(CCC)[C@@H]1Cc2c(I)ccc3c2[C@@H](C1)CN3C(=O)c1ccccc1.CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ncco1>C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.C1(=CC=CC=C1)C>CCCN(CCC)[C@@H]1Cc2c(-c3ncco3)ccc3c2...
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ac7194da57c94ba59ea021918cf5a3f6
CC(=O)c1ccc2c3c1C[C@@H](N(CC1CC1)CC1CC1)C[C@H]3CN2.O=C(Cl)OCC(Cl)(Cl)Cl>>NC(=O)N1CCc2ccccc21
C(C)(=O)C1=C2C=3[C@H](CNC3C=C1)C[C@@H](C2)N(CC2CC2)CC2CC2.C(C)N(CC)CC.ClC(COC(=O)Cl)(Cl)Cl>>C(N)(=O)N1CCC2=CC=CC=C12
CC(=O)[c:9]1[c:8]2[c:7]3[c:12]([cH:11][cH:10]1)[NH:4][CH2:5][C@@H:6]3C[C@H](N(CC1CC1)CC1CC1)C2.ClC(Cl)(Cl)CO[C:2](Cl)=[O:3]>>[NH2:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]21
CC(=O)c1ccc2c3c1C[C@@H](N(CC1CC1)CC1CC1)C[C@H]3CN2.O=C(Cl)OCC(Cl)(Cl)Cl
NC(=O)N1CCc2ccccc21
null
null
C(Cl)Cl
Acylation
OtherReaction
cfef4e5e5fdae48f59ad6869f2f439a4028225831e19761cbc31175326d5e356
1fea30f316824198e233dc7d7d5f0ed1a4a322c4c89c24d4336ce38c6250dbb8
c1ccc2c(c1)CCN2
null
248.2
[{"value": 248.2, "product": "C(N)(=O)N1CCC2=CC=CC=C12", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of (-)(2aR,4S)-6-acetyl-4-[di-(cyclopropylmethyl)amino]-1,2,2a, 3,4,5-hexahydrobenz-[cd]indole (2.5 g, 7.7 mmol) and triethylamine (1.1 ml, 8 mmol) in 90 ml CH2Cl2 was added dropwise a solution of 2,2,2-trichloroethylchloroformate (1.7 g, 8 mmol) in 10 ml CH2Cl2. The reaction mixture was stirred at room t...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Trichloro group.Ketone.Ether.Secondary amine.Tertiary amine
Urea
c1cc2c3c(c1)NC[C@@H]3CCC2.C1CC1.C1CC1
c1ccc2c(c1)CC[NH]2
c1ccc2c(c1)CC[NH]2
HCl
C(Cl)Cl
null
1
CC(=O)c1ccc2c3c1C[C@@H](N(CC1CC1)CC1CC1)C[C@H]3CN2.O=C(Cl)OCC(Cl)(Cl)Cl>C(Cl)Cl>NC(=O)N1CCc2ccccc21
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-967d5eaacb4f4440a0cdf06e4362297a
CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@@H](C1)CN3C(=O)c1ccccc1>>CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@H](CN3)C1
Cl.C(CCC)[Li].C(C1=CC=CC=C1)(=O)N1C[C@H]2C=3C(=C(C=CC13)Br)C[C@H](C2)N(CCC)CCC>>BrC1=C2C=3[C@H](CNC3C=C1)C[C@@H](C2)N(CCC)CCC
O=C(c1ccccc1)[N:19]1[c:15]2[cH:14][cH:13][c:11]([Br:12])[c:10]3[c:16]2[C@H:17]([CH2:18]1)[CH2:20][C@H:8]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH2:6][CH3:7])[CH2:9]3>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7])[C@@H:8]1[CH2:9][c:10]2[c:11]([Br:12])[cH:13][cH:14][c:15]3[c:16]2[C@H:17]([CH2:18][NH:19]3)[CH2:20]1
CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@@H](C1)CN3C(=O)c1ccccc1
CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@H](CN3)C1
null
null
O1CCCC1.CCCCCC
Reduction
Hydrogenolysis of tertiary amines
f45e448ff068294d2c8d3a9f528f91025783a450ab56031bb2e90a884f88ae9e
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
c1cc2c3c(c1)NC[C@@H]3CCC2
O=C(-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[c:4]:[c:5]-1:[c:6])-c1:c:c:c:c:c:1>>[c:6]:[c:5]1:[c:4]-[C:3]-[C:2]-[NH;D2;+0:1]-1
98.1
[{"value": 98.1, "product": "BrC1=C2C=3[C@H](CNC3C=C1)C[C@@H](C2)N(CCC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
30
MINUTE
To a stirred solution of 12.8 g (29 mmol) of (+)(2aR,4S)-1-benzoyl-6-bromo-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole in 200 ml of tetrahydrofuran cooled to -78° C. under a nitrogen atmosphere was added 20 ml (32 mmol) of a 1.6M solution of n-butyllithium in hexane. The reaction mixture was stirred at -7...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccccc1.c1cc2c3c(c1)[NH]C[C@@H]3CCC2
c1cc2c3c(c1)NC[C@@H]3CCC2
c1cc2c3c(c1)NC[C@@H]3CCC2
HO-
O1CCCC1.CCCCCC
-78
0.5
CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@@H](C1)CN3C(=O)c1ccccc1>O1CCCC1.CCCCCC>CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@H](CN3)C1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ceac2350ec8e4ed58bf37324a62946d8
CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1.CN(C)C=O>>CCCN(CCC)[C@@H]1Cc2c(C=O)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1
CN(C=O)C.C(CCC)[Li].BrC1=C2C=3[C@H](CN(C3C=C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C[C@@H](C2)N(CCC)CCC>>C(=O)C1=C2C=3[C@H](CN(C3C=C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C[C@@H](C2)N(CCC)CCC
Br[c:11]1[c:10]2[c:17]3[c:16]([cH:15][cH:14]1)[N:21]([C:22]([c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1)([c:29]1[cH:30][cH:31][cH:32][cH:33][cH:34]1)[c:35]1[cH:36][cH:37][cH:38][cH:39][cH:40]1)[CH2:20][C@@H:18]3[CH2:19][C@H:8]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH2:6][CH3:7])[CH2:9]2.CN(C)[CH:12]=[O:13]>>[CH3:1][CH2:2...
CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1.CN(C)C=O
CCCN(CCC)[C@@H]1Cc2c(C=O)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1
null
null
O1CCCC1.CCCCCC
C-C Coupling
Bouveault aldehyde synthesis
a9aba44afaf7ca85d37196ef805393b43ce7e6c47fe83d78da3f1131444f7a27
afd09ced98f25d311f21cc04ba6a50fe7e5516de47e17484683ded13d323b1b2
c1ccc(C(c2ccccc2)(c2ccccc2)N2C[C@@H]3CCCc4cccc2c43)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5])-[C:6].C-N(-C)-[CH;D2;+0:7]=[O;D1;H0:8]>>[C:6]-[c:4](:[c:5]):[c;H0;D3;+0:1](-[CH;D2;+0:7]=[O;D1;H0:8]):[c:2]:[c:3]
null
[]
-78
CELSIUS
1
HOUR
To a solution of (-)(2aR,4S)-6-bromo-1-trityl-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole (6.8 g, 12 mmol) in 100 ml of tetrahydrofuran cooled to -78° C. under a nitrogen atmosphere was added dropwise a 1.6M solution of n-butyllithium in hexane. The reaction mixture was stirred at -78° C. for 1 hour. Dime...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tertiary amide
Aldehyde
c1cc2c3c(c1)[NH]C[C@@H]3CCC2
c1cc2c3c(c1)[NH]C[C@@H]3CCC2
c1cc2c3c(c1)[NH]C[C@@H]3CCC2.c1ccccc1.c1ccccc1.c1ccccc1
HBr
O1CCCC1.CCCCCC
-78
1
CCCN(CCC)[C@@H]1Cc2c(Br)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1.CN(C)C=O>O1CCCC1.CCCCCC>CCCN(CCC)[C@@H]1Cc2c(C=O)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d7e915c839664651bb5e7f91dffd18da
CCCN(CCC)[C@@H]1Cc2c(C=O)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1.[C-]#[N+]CS(=O)(=O)c1ccc(C)cc1>>CCCN(CCC)[C@@H]1Cc2c(-c3cnco3)ccc3c2[C@H](CN3)C1
C(=O)C1=C2C=3[C@H](CN(C3C=C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C[C@@H](C2)N(CCC)CCC.S(=O)(=O)(C1=CC=C(C)C=C1)C[N+]#[C-].C([O-])([O-])=O.[K+].[K+]>>O1C=NC=C1C1=C2C=3[C@H](CNC3C=C1)C[C@@H](C2)N(CCC)CCC
c1ccc(C(c2ccccc2)(c2ccccc2)[N:23]2[c:19]3[cH:18][cH:17][c:11]([CH:12]=[O:16])[c:10]4[c:20]3[C@H:21]([CH2:22]2)[CH2:24][C@H:8]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH2:6][CH3:7])[CH2:9]4)cc1.Cc1ccc(S(=O)(=O)[CH2:13][N+:14]#[C-:15])cc1>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7])[C@@H:8]1[CH2:9][c:10]2[c:11](-[c:12]...
CCCN(CCC)[C@@H]1Cc2c(C=O)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1.[C-]#[N+]CS(=O)(=O)c1ccc(C)cc1
CCCN(CCC)[C@@H]1Cc2c(-c3cnco3)ccc3c2[C@H](CN3)C1
null
null
CO
Functional Group Interconversion
OtherReaction
a52408565944c7a3d1c1a7743313d56487f881a8ffbe35500dfc713845dcf304
81799e45ca88af47fd09bd6e38a4dacf267ea894a887436deadef53d6689f76a
c1ncc(-c2ccc3c4c2CCC[C@H]4CN3)o1
C-c1:c:c:c(-S(=O)(=O)-[CH2;D2;+0:1]-[N+;H0;D2:2]#[C-;H0;D1:3]):c:c:1.[C:4]-[c:5]1:[c:6]2:[c:7](:[c:8]:[c:9]:[c;H0;D3;+0:10]:1-[CH;D2;+0:11]=[O;H0;D1;+0:12])-[N;H0;D3;+0:13](-C(-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1)-[C:14]-[C:15]-2>>[C:4]-[c:5]1:[c:6]2:[c:7](:[c:8]:[c:9]:[c;H0;D3;+0:10]:1-[c;H0;D3;+0:11]1:[cH...
153.6
[{"value": 153.6, "product": "O1C=NC=C1C1=C2C=3[C@H](CNC3C=C1)C[C@@H](C2)N(CCC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A reaction mixture of (-)(2aR,4S)-6-formyl-1-trityl-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole (1.06 g, 2 mmol), tosylmethyl isocyanide (390 mg, 2 mmol) and potassium carbonate (304 mg, 2.2 imnol) in 100 ml of methanol was stirred at reflux temperature under a nitrogen atomosphere for 16 hours. The react...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Aldehyde.Isocyanide.Tertiary amine
Secondary amine
c1ccccc1.c1ccccc1.c1ccccc1.c1cc2c3c(c1)[NH]C[C@@H]3CCC2.c1ccccc1
c1cocn1.c1cc2c3c(c1)NC[C@@H]3CCC2
c1cocn1.c1cc2c3c(c1)NC[C@@H]3CCC2
TsOH.HO-
CO
null
null
CCCN(CCC)[C@@H]1Cc2c(C=O)ccc3c2[C@@H](C1)CN3C(c1ccccc1)(c1ccccc1)c1ccccc1.[C-]#[N+]CS(=O)(=O)c1ccc(C)cc1>CO>CCCN(CCC)[C@@H]1Cc2c(-c3cnco3)ccc3c2[C@H](CN3)C1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ed13c97cbeb948bda6aee994a95925f6
Brc1cccnc1>>OB(O)c1cccnc1
BrC=1C=NC=CC1.COB(OC)OC.C(C)(C)(C)[Li]>>N1=CC(=CC=C1)B(O)O
Br[c:4]1[cH:5][cH:6][cH:7][n:8][cH:9]1>>[OH:1][B:2]([OH:3])[c:4]1[cH:5][cH:6][cH:7][n:8][cH:9]1
Brc1cccnc1
OB(O)c1cccnc1
null
null
CCCCC.C(C)OCC
Functional Group Interconversion
Preparation of boronic acids without boronic ether
3924fd76fbdecc276cb0ec82b47a9205afc0daae8b87f757779433597cbd5b83
3c67ef5cce82b121a680ae296eb1f6d78abe8f9494b62ca3b872477b7553bcfd
c1ccncc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1>>[O;D1;H1:7]-[#5:8](-[O;D1;H1:9])-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1
null
[]
null
null
null
null
A solution of 4.0 ml (6.56 g, 42 mmol) of 3-bromopyridine and 9 ml (8 mmol) of trimethylborate in 100 ml of diethyl ether was cooled to -70° C. then treated slowly with 33 ml (83.8 mmol) of a 2.54M tert-butyllithium in pentane solution. After allowing the resulting slurry to warm to room temperature the solvents were e...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Boronic acid
c1ccncc1
c1ccncc1
c1ccncc1
Br-
CCCCC.C(C)OCC
null
null
Brc1cccnc1>CCCCC.C(C)OCC>OB(O)c1cccnc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-122a417cbb4b4aedbca3470d47e02bd4
CCCCC[C@@H]1CC[C@@H](C(=O)O)CC1.C[C@@H](O)[C@@H](N)C(=O)O>>CCCCC[C@@H]1CC[C@@H](C(=O)N[C@@H](C(=O)O)[C@@H](C)O)CC1
C(CCCC)[C@@H]1CC[C@H](CC1)C(=O)O.C(C(=O)Cl)(=O)Cl.N[C@H]([C@H](O)C)C(=O)O.[OH-].[Na+]>>C(CCCC)[C@@H]1CC[C@H](CC1)C(=O)N[C@H]([C@H](O)C)C(=O)O
O[C:10]([C@H:9]1[CH2:8][CH2:7][C@H:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])[CH2:21][CH2:20]1)=[O:11].[NH2:12][C@@H:13]([C:14](=[O:15])[OH:16])[C@@H:17]([CH3:18])[OH:19]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[CH2:7][CH2:8][C@H:9]([C:10](=[O:11])[NH:12][C@@H:13]([C:14](=[O:15])[OH:16])[C@@H:17]([CH3:18])[OH:19])[CH2...
CCCCC[C@@H]1CC[C@@H](C(=O)O)CC1.C[C@@H](O)[C@@H](N)C(=O)O
CCCCC[C@@H]1CC[C@@H](C(=O)N[C@@H](C(=O)O)[C@@H](C)O)CC1
null
null
C(C)#N.C1(=CC=CC=C1)C.C1CCOC1
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
C1CCCCC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5].[C:6]-[C:7](-[NH2;D1;+0:8])-[C:9](=[O;D1;H0:10])-[O;D1;H1:11]>>[C:6]-[C:7](-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5])-[C:9](=[O;D1;H0:10])-[O;D1;H1:11]
null
[]
null
null
1
HOUR
A solution of trans-4-pentylcyclohexane carboxylic acid (198 mg, 1.0 mmol) in dry toluene (1 mL) is treated with oxalyl chloride (760 mg, 5.9 mmol) at 0° C. and the mixture is stirred for 2 h at the same temperature and 1 h at room temperature. Excess reagent is removed in vacuo. A solution of the crude acid chloride i...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
C1CCCCC1
HO-
C(C)#N.C1(=CC=CC=C1)C.C1CCOC1
null
1
CCCCC[C@@H]1CC[C@@H](C(=O)O)CC1.C[C@@H](O)[C@@H](N)C(=O)O>C(C)#N.C1(=CC=CC=C1)C.C1CCOC1>CCCCC[C@@H]1CC[C@@H](C(=O)N[C@@H](C(=O)O)[C@@H](C)O)CC1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-f4490b4e928e4b9d9dcb6defa9a6ab99
CCCCOc1ccc(CC(=O)O)cc1.C[C@@H](O)[C@@H](N)C(=O)O>>CCCCOc1ccc(CC(=O)N[C@@H](C(=O)O)[C@@H](C)O)cc1
C(CCC)OC1=CC=C(C=C1)CC(=O)O.N[C@H]([C@H](O)C)C(=O)O>>C(CCC)OC1=CC=C(C=C1)CC(=O)N[C@H]([C@H](O)C)C(=O)O
O[C:11]([CH2:10][c:9]1[cH:8][cH:7][c:6]([O:5][CH2:4][CH2:3][CH2:2][CH3:1])[cH:22][cH:21]1)=[O:12].[NH2:13][C@@H:14]([C:15](=[O:16])[OH:17])[C@@H:18]([CH3:19])[OH:20]>>[CH3:1][CH2:2][CH2:3][CH2:4][O:5][c:6]1[cH:7][cH:8][c:9]([CH2:10][C:11](=[O:12])[NH:13][C@@H:14]([C:15](=[O:16])[OH:17])[C@@H:18]([CH3:19])[OH:20])[cH:21...
CCCCOc1ccc(CC(=O)O)cc1.C[C@@H](O)[C@@H](N)C(=O)O
CCCCOc1ccc(CC(=O)N[C@@H](C(=O)O)[C@@H](C)O)cc1
null
null
null
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4].[C:5]-[C:6](-[NH2;D1;+0:7])-[C:8](=[O;D1;H0:9])-[O;D1;H1:10]>>[C:5]-[C:6](-[NH;D2;+0:7]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4])-[C:8](=[O;D1;H0:9])-[O;D1;H1:10]
null
[]
null
null
null
null
4-Butoxyphenylacetic acid (288 mg, 1.38 mmol) is converted to the acid chloride and added to D-allo-Thr (150 mg, 1.26 mmol) to get 2c-9, following the procedure described in Example 6. The crude product is purified by chromatography (2.5×18 cm column, gradient 4% CH3OH and 0.3% HOAc in CH2Cl2): NMR δ 0.96 (t, J=7.4, 3 ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1
HO-
null
null
null
CCCCOc1ccc(CC(=O)O)cc1.C[C@@H](O)[C@@H](N)C(=O)O>>CCCCOc1ccc(CC(=O)N[C@@H](C(=O)O)[C@@H](C)O)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-fab0c7f6479240acbdfc8fbbda591dda
COC(=O)C(CCC[C@@H](NC(=O)OC(C)(C)C)C(=O)N[C@H](C)C(=O)OCc1ccc([N+](=O)[O-])cc1)NC(=O)OCc1ccccc1.OCc1ccccc1>>C[C@@H](NC(=O)[C@@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C)C(=O)OCc1ccccc1
[N+](=O)([O-])C1=CC=C(C=C1)COC([C@H](NC([C@H](NC(=O)OC(C)(C)C)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OC)=O)C)=O.C(C1=CC=CC=C1)O>>C1(=CC=CC=C1)COC([C@H](NC([C@H](NC(=O)OC(C)(C)C)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O
CO[C:22]([CH:10]([CH2:9][CH2:8][CH2:7][C@H:6]([C:4]([NH:3][C@H:2]([CH3:1])[C:40](=[O:41])[O:42][CH2:43][c:44]1[cH:45][cH:46][c:47]([N+](=O)[O-])[cH:48][cH:49]1)=[O:5])[NH:32][C:33](=[O:34])[O:35][C:36]([CH3:37])([CH3:38])[CH3:39])[NH:11][C:12](=[O:13])[O:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1)=[O:23].[O...
COC(=O)C(CCC[C@@H](NC(=O)OC(C)(C)C)C(=O)N[C@H](C)C(=O)OCc1ccc([N+](=O)[O-])cc1)NC(=O)OCc1ccccc1.OCc1ccccc1
C[C@@H](NC(=O)[C@@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C)C(=O)OCc1ccccc1
null
CC([O-])C.[Ti+4].CC([O-])C.CC([O-])C.CC([O-])C
C1CCOC1
Acylation
OtherReaction
67a2521538f1cf3882205adfab927bff9f52a980468c3c6e198dddc2fc57a40d
8028bfd6e276cc9541453e1ce714c6ecfffcc714d2893f27985288769ccd7d51
O=C(CCCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)NCC(=O)OCc1ccccc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[#7:5]-[C:6]=[O;D1;H0:7].O=[N+](-[O-])-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12].[OH;D1;+0:13]-[C:14]-[c:15]>>[C:4]-[C:3](-[#7:5]-[C:6]=[O;D1;H0:7])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[O;H0;D2;+0:13]-[C:14]-[c:15].[c:10]:[c:9]:[cH;D2;+0:8]:[c:11]:[c:12]
88.4
[{"value": 88.0, "product": "C1(=CC=CC=C1)COC([C@H](NC([C@H](NC(=O)OC(C)(C)C)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 88.4, "product": "C1(=CC=CC=C1)COC([C@H](NC([C@H](NC(=O)OC(C)(C)C)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O", "details":...
null
null
30
MINUTE
A mixture of N-[N2 -[(1,1-dimethylethoxy)carbonyl]-N6-[(phenylmethoxy)-carbonyl]-(R)-6-[(methoxy)carbonyl]-L-lysyl]-D-alanine 4-nitrophenylmethyl ester (40a, Kolodziejczyk, et. al., Int. J. Pept. Prot. Res., 1992, 39, 382; 683 mg, 1.06 mmol), 4-- molecular sieves (2.15 g, crushed), THF (10.5 mL), and benzyl alcohol (11...
10.6084/m9.figshare.5104873.v1
null
Ester.Nitro group.Primary alcohol
Ester
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1
HO-
CC([O-])C.[Ti+4].CC([O-])C.CC([O-])C.CC([O-])C.C1CCOC1
null
0.5
COC(=O)C(CCC[C@@H](NC(=O)OC(C)(C)C)C(=O)N[C@H](C)C(=O)OCc1ccc([N+](=O)[O-])cc1)NC(=O)OCc1ccccc1.OCc1ccccc1>CC([O-])C.[Ti+4].CC([O-])C.CC([O-])C.CC([O-])C.C1CCOC1>C[C@@H](NC(=O)[C@@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C)C(=O)OCc1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a7bbe3157e2343b29b5ae2259a7f0280
C[C@@H](NC(=O)[C@@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C)C(=O)OCc1ccccc1>>C[C@@H](NC(=O)[C@H](N)CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)OCc1ccccc1
C1(=CC=CC=C1)COC([C@H](NC([C@H](NC(=O)OC(C)(C)C)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O>>C1(=CC=CC=C1)COC([C@H](NC([C@H](N)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O
CC(C)(C)OC(=O)[NH:7][C@@H:6]([C:4]([NH:3][C@H:2]([CH3:1])[C:33](=[O:34])[O:35][CH2:36][c:37]1[cH:38][cH:39][cH:40][cH:41][cH:42]1)=[O:5])[CH2:8][CH2:9][CH2:10][CH:11]([NH:12][C:13](=[O:14])[O:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[C:23](=[O:24])[O:25][CH2:26][c:27]1[cH:28][cH:29][cH:30][cH:31][cH:32]1>...
C[C@@H](NC(=O)[C@@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C)C(=O)OCc1ccccc1
C[C@@H](NC(=O)[C@H](N)CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)OCc1ccccc1
null
null
C(=O)(C(F)(F)F)O
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=C(CCCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)NCC(=O)OCc1ccccc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4](=[O;D1;H0:5])-[#7:6]-[C:7]-[C:8](-[#8:9])=[O;D1;H0:10]>>[#8:9]-[C:8](=[O;D1;H0:10])-[C:7]-[#7:6]-[C:4](=[O;D1;H0:5])-[C:2](-[C:3])-[NH2;D1;+0:1]
105.6
[{"value": 105.6, "product": "C1(=CC=CC=C1)COC([C@H](NC([C@H](N)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 40b (251 mg, 0.37 mmol) in TFA (870 μl) is stirred for 30 min at 0° C. The TFA is removed and the oil is taken up in EtOAc and washed with saturated NaHCO3 solution. Drying and removal of the solvent gives 3b (225 mg, slight excess) which is used in subsequent reactions without further handling: NMR δ 1.3...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(=O)(C(F)(F)F)O
null
null
C[C@@H](NC(=O)[C@@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C)C(=O)OCc1ccccc1>C(=O)(C(F)(F)F)O>C[C@@H](NC(=O)[C@H](N)CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)OCc1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d896f7bdfcab4970950d4d3e8a62ba2c
CCCCCCC(=O)N[C@@H](C(=O)OCc1ccccc1)[C@@H](C)O.C[C@@H](NC(=O)[C@H](N)CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)OCc1ccccc1.O=C(Cl)Cl>>CCCCCCC(=O)NC(C(=O)OCc1ccccc1)C(C)OC(=O)N[C@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OCc1ccccc1
C1(=CC=CC=C1)COC([C@H](NC(CCCCCC)=O)[C@H](O)C)=O.C(=O)(Cl)Cl.C1(=CC=CC=C1)COC([C@H](NC([C@H](N)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O>>C1(=CC=CC=C1)COC([C@H](NC([C@H](NC(=O)OC(C(C(OCC1=CC=CC=C1)=O)NC(CCCCCC)=O)C)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[NH:9][C@@H:10]([C:11](=[O:12])[O:13][CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1)[C@@H:21]([CH3:22])[OH:23].[NH2:26][C@H:27]([CH2:28][CH2:29][CH2:30][CH:31]([NH:32][C:33](=[O:34])[O:35][CH2:36][c:37]1[cH:38][cH:39][cH:40][cH:41][cH:42]1)[C:43](=[O:44])[O:45...
CCCCCCC(=O)N[C@@H](C(=O)OCc1ccccc1)[C@@H](C)O.C[C@@H](NC(=O)[C@H](N)CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)OCc1ccccc1.O=C(Cl)Cl
CCCCCCC(=O)NC(C(=O)OCc1ccccc1)C(C)OC(=O)N[C@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OCc1ccccc1
null
null
CCOC(=O)C.O.CC#N.C1CCOC1
Protection
OtherReaction
3d68f0bb52b2df855222c8931b2a71f964865ce2ec96df1e3152c2a869e9cad1
c63e4fd0e0f3664367af6bef32d20900630deacde56a2d0fc4d3ba46b7f4728b
O=C(CCOC(=O)N[C@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)NCC(=O)OCc1ccccc1)OCc1ccccc1
Cl-[C;H0;D3;+0:1](-Cl)=[O;D1;H0:2].[#8:3]-[C:4](=[O;D1;H0:5])-[C:6]-[#7:7]-[C:8](=[O;D1;H0:9])-[C:10](-[C:11])-[NH2;D1;+0:12].[C:13]-[#8:14]-[C:15](=[O;D1;H0:16])-[C:17](-[#7:18]-[C:19]=[O;D1;H0:20])-[C@@H;D3;+0:21](-[C;D1;H3:22])-[OH;D1;+0:23]>>[#8:3]-[C:4](=[O;D1;H0:5])-[C:6]-[#7:7]-[C:8](=[O;D1;H0:9])-[C:10](-[C:11]...
null
[]
null
null
5
HOUR
A solution of 2e-1 (173.6 mg, 0.54 mmol) in THF (Sure/Seal solvent redried over 3--MS, 1.45 mL) is added to excess cold phosgene (1.92M solution in toluene; 1.40 mL, 2.63 mmol), alternately with TEA (81 μl, 0.58 mmol) over a period of 15 min at 0° C. The resulting milky mixture is stirred for an addition 15 min at the ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Secondary alcohol.Primary amine
Carbamic ester
null
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HCl
CCOC(=O)C.O.CC#N.C1CCOC1
null
5
CCCCCCC(=O)N[C@@H](C(=O)OCc1ccccc1)[C@@H](C)O.C[C@@H](NC(=O)[C@H](N)CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)OCc1ccccc1.O=C(Cl)Cl>CCOC(=O)C.O.CC#N.C1CCOC1>CCCCCCC(=O)NC(C(=O)OCc1ccccc1)C(C)OC(=O)N[C@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OCc1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-47bad7a88d7c419c9e60e8abe49c3d77
CCCCCCC(=O)NC(C(=O)OCc1ccccc1)C(C)OC(=O)N[C@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OCc1ccccc1>>CCCCCCC(=O)NC(C(=O)O)C(C)OC(=O)N[C@H](CCCC(N)C(=O)O)C(=O)N[C@H](C)C(=O)O
C1(=CC=CC=C1)COC([C@H](NC([C@H](NC(=O)OC(C(C(OCC1=CC=CC=C1)=O)NC(CCCCCC)=O)C)CCCC(NC(=O)OCC1=CC=CC=C1)C(=O)OCC1=CC=CC=C1)=O)C)=O>>C(=O)(O)C(CCC[C@@H](NC(=O)OC(C(NC(CCCCCC)=O)C(=O)O)C)C(=O)N[C@H](C)C(=O)O)N
O=C(OCc1ccccc1)[NH:25][CH:24]([CH2:23][CH2:22][CH2:21][C@@H:20]([NH:19][C:17]([O:16][CH:14]([CH:10]([NH:9][C:7]([CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])=[O:8])[C:11](=[O:12])[O:13]Cc1ccccc1)[CH3:15])=[O:18])[C:29](=[O:30])[NH:31][C@H:32]([CH3:33])[C:34](=[O:35])[O:36]Cc1ccccc1)[C:26](=[O:27])[O:28]Cc1ccccc1>>[CH3:1]...
CCCCCCC(=O)NC(C(=O)OCc1ccccc1)C(C)OC(=O)N[C@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OCc1ccccc1
CCCCCCC(=O)NC(C(=O)O)C(C)OC(=O)N[C@H](CCCC(N)C(=O)O)C(=O)N[C@H](C)C(=O)O
null
[OH-].[OH-].[Pd+2]
CCOC(=O)C.CCO
Reduction
OtherReaction
93f12f53ec8755e6497c80a0567af4871fd2a985c1b630f3d409d24de7706e58
f7527cac2ca4830281723fda6ba4921ecc42f4fadea8f894a8ccad6b4c927d07
null
O=C(-O-C-c1:c:c:c:c:c:1)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4](=[O;D1;H0:5])-[O;H0;D2;+0:6]-C-c1:c:c:c:c:c:1.[C:7]-[C:8](=[O;D1;H0:9])-[O;H0;D2;+0:10]-C-c1:c:c:c:c:c:1.[C:11]-[C:12](=[O;D1;H0:13])-[O;H0;D2;+0:14]-C-c1:c:c:c:c:c:1>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4](=[O;D1;H0:5])-[OH;D1;+0:6].[C:7]-[C:8](=[O;D1;H0:9])-[OH;D1;...
null
[]
null
null
5.5
HOUR
A solution of 1a-1 (140 mg, 0.15 mmol) in EtOAc/EtOH (5 mL:15 mL) is hydrogenated over Pd(OH)2 (Pearlman's catalyst, 20% on C, 100 mg) using a Parr apparatus at an initial pressure of 70 psi. After 5.5 h, filtration and evaporation gives a colorless glass. The latter is triturated with ether and the sides of the flask ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ester.Ester.Ester.Ether
Carboxylic acid.Carboxylic acid.Carboxylic acid.Primary amine
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
null
null
HO-
[OH-].[OH-].[Pd+2].CCOC(=O)C.CCO
null
5.5
CCCCCCC(=O)NC(C(=O)OCc1ccccc1)C(C)OC(=O)N[C@H](CCCC(NC(=O)OCc1ccccc1)C(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OCc1ccccc1>[OH-].[OH-].[Pd+2].CCOC(=O)C.CCO>CCCCCCC(=O)NC(C(=O)O)C(C)OC(=O)N[C@H](CCCC(N)C(=O)O)C(=O)N[C@H](C)C(=O)O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-fc79242360f14622a6a0957e5c6bd892
CCCCCC.CCCCCCC(=O)N[C@@H](CO)C(=O)OC.CCOC(C)=O>>CCCCCCC(=O)N1[C@H](C(=O)OC)COC1(C)C
COC([C@@H](NC(CCCCCC)=O)CO)=O.CC=1C=CC(=CC1)S(=O)(=O)O.CCCCCC.CCOC(=O)C.C(=O)([O-])[O-].[K+].[K+]>>COC(=O)[C@H]1N(C(OC1)(C)C)C(CCCCCC)=O
CCCCC[CH3:19].[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[NH:9][C@H:10]([C:11](=[O:12])[O:13][CH3:14])[CH2:15][OH:16].CCO[C:17](=O)[CH3:18]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[N:9]1[C@H:10]([C:11](=[O:12])[O:13][CH3:14])[CH2:15][O:16][C:17]1([CH3:18])[CH3:19]
CCCCCC.CCCCCCC(=O)N[C@@H](CO)C(=O)OC.CCOC(C)=O
CCCCCCC(=O)N1[C@H](C(=O)OC)COC1(C)C
null
null
CC(=O)C.COC(C)(C)OC
Heteroatom Alkylation and Arylation
OtherReaction
710a85dd6a91fbf39b6013ce9cdafa1daab72f8b8adcb5ec399f373d14fe75f9
567a9783e07a178d793aef6ce57238f12658c3c2aa08cc932125383868d3d685
C1COCN1
C-C-C-C-C-[CH3;D1;+0:1].C-C-O-[C;H0;D3;+0:2](=O)-[C;D1;H3:3].[C:4]-[C:5](=[O;D1;H0:6])-[NH;D2;+0:7]-[C:8](-[C:9]-[OH;D1;+0:10])-[C:11](=[O;D1;H0:12])-[#8:13]-[C;D1;H3:14]>>[C:4]-[C:5](=[O;D1;H0:6])-[N;H0;D3;+0:7]1-[C:8](-[C:11](=[O;D1;H0:12])-[#8:13]-[C;D1;H3:14])-[C:9]-[O;H0;D2;+0:10]-[C;H0;D4;+0:2]-1(-[C;D1;H3:3])-[C...
null
[]
null
null
null
null
Compound 2j (320 mg, 1.38 mmol) and p-TSA (40 mg) are dissolved in dry acetone (2 ml) and 2,2-dimethoxypropane (2 ml). The resulting solution is heated overnight at reflux. Solid K2CO3 is added and the volatiles removed in vacuo to give a residue. Flash chromatography (2×21 cm column, 6:1 hexane/EtOAc) of the residue p...
10.6084/m9.figshare.5104873.v1
null
Ester.Secondary amide.Primary alcohol
Ether.Tertiary amide
null
C1COC[NH]1
C1COC[NH]1
HO-
CC(=O)C.COC(C)(C)OC
null
null
CCCCCC.CCCCCCC(=O)N[C@@H](CO)C(=O)OC.CCOC(C)=O>CC(=O)C.COC(C)(C)OC>CCCCCCC(=O)N1[C@H](C(=O)OC)COC1(C)C
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-6be7cdeeabcd409597ffca3d172897d1
CCCCCCC(=O)N1[C@H](C(=O)OC)COC1(C)C>>CCCCCCC(=O)N1[C@H](CO)COC1(C)C
COC(=O)[C@H]1N(C(OC1)(C)C)C(CCCCCC)=O.[BH4-].[Li+]>>CC1(OC[C@H](N1C(CCCCCC)=O)CO)C
CO[C:11]([C@H:10]1[N:9]([C:7]([CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])=[O:8])[C:15]([CH3:16])([CH3:17])[O:14][CH2:13]1)=[O:12]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[N:9]1[C@H:10]([CH2:11][OH:12])[CH2:13][O:14][C:15]1([CH3:16])[CH3:17]
CCCCCCC(=O)N1[C@H](C(=O)OC)COC1(C)C
CCCCCCC(=O)N1[C@H](CO)COC1(C)C
null
null
CCOCC
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
C1COCN1
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]1-[C:4]-[#8:5]-[C:6]-[#7:7]-1-[C:8]=[O;D1;H0:9]>>[O;D1;H0:9]=[C:8]-[#7:7]1-[C:6]-[#8:5]-[C:4]-[C:3]-1-[CH2;D2;+0:1]-[OH;D1;+0:2]
null
[]
null
null
3
HOUR
A solution of 8a (296 mg, 1.09 mmol) in dry ether (1 mL) is treated with lithium borohydride (2M solution in THF, 0.55 mL, 1.09 meq) under an argon atmosphere. The mixture is stirred for 3 hr at reflux and 18 h at room temperature. The resulting mixture is diluted with ether and quenched with methanol. The volatiles ar...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
C1COC[NH]1
Other
CCOCC
null
3
CCCCCCC(=O)N1[C@H](C(=O)OC)COC1(C)C>CCOCC>CCCCCCC(=O)N1[C@H](CO)COC1(C)C
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-cd0d169049644f7aa72f8fc73856b15d
CCCCCCC(=O)N1[C@H](CO)COC1(C)C>>CCCCCCC(=O)N1[C@H](C=O)COC1(C)C
C(C)N(CC)CC.CC1(OC[C@H](N1C(CCCCCC)=O)CO)C.C(C(=O)Cl)(=O)Cl.CS(=O)C>>CC1(OC[C@H](N1C(CCCCCC)=O)C=O)C
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[N:9]1[C@H:10]([CH2:11][OH:12])[CH2:13][O:14][C:15]1([CH3:16])[CH3:17]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[N:9]1[C@H:10]([CH:11]=[O:12])[CH2:13][O:14][C:15]1([CH3:16])[CH3:17]
CCCCCCC(=O)N1[C@H](CO)COC1(C)C
CCCCCCC(=O)N1[C@H](C=O)COC1(C)C
null
null
O.C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
C1COCN1
[O;D1;H0:1]=[C:2]-[#7:3]1-[C:4]-[#8:5]-[C:6]-[C:7]-1-[CH2;D2;+0:8]-[OH;D1;+0:9]>>[O;D1;H0:1]=[C:2]-[#7:3]1-[C:4]-[#8:5]-[C:6]-[C:7]-1-[CH;D2;+0:8]=[O;H0;D1;+0:9]
null
[]
-60
CELSIUS
15
MINUTE
A solution of oxalyl chloride (105 μl, 1.23 mmol) in CH2Cl2 (2.75 mL) is cooled to -60° C. A solution of DMSO (192 μL) in CH2Cl2 (0.55 mL) is added over a period of 5 min. and the resulting milky mixture is stirred for 15 min at -60° C. The alcohol from Example 39 (133 mg., 0.55 mmol) in CH2Cl2 (0.55 ml) is added to th...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
C1COC[NH]1
null
O.C(Cl)Cl
-60
0.25
CCCCCCC(=O)N1[C@H](CO)COC1(C)C>O.C(Cl)Cl>CCCCCCC(=O)N1[C@H](C=O)COC1(C)C
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ba83b90f82aa43f2bdb332b49d366c08
CCCCCCC(=O)N1[C@H](C=O)COC1(C)C>>CCCCCCC(=O)N1[C@H](C(O)CC)COC1(C)C
CC1(OC[C@H](N1C(CCCCCC)=O)C=O)C.CC[Mg+].[Br-]>>C(C)C(O)[C@H]1N(C(OC1)(C)C)C(CCCCCC)=O
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[N:9]1[C@H:10]([CH:11]=[O:12])[CH2:15][O:16][C:17]1([CH3:18])[CH3:19]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[N:9]1[C@H:10]([CH:11]([OH:12])[CH2:13][CH3:14])[CH2:15][O:16][C:17]1([CH3:18])[CH3:19]
CCCCCCC(=O)N1[C@H](C=O)COC1(C)C
CCCCCCC(=O)N1[C@H](C(O)CC)COC1(C)C
null
null
CCOCC
Miscellaneous
OtherReaction
1ffaf80f172e20da969364a5d2977299bc51b204f2262675c45c8ec58ff36ac0
e005d650d08e61fc67b766830eb53235a9bc084cc3667d2f8a73c2fb8bb34277
C1COCN1
[O;D1;H0:1]=[C:2]-[#7:3]1-[C:4]-[#8:5]-[C:6]-[C:7]-1-[CH;D2;+0:8]=[O;H0;D1;+0:9]>>[C;D1;H3:10]-[C:11]-[CH;D3;+0:8](-[OH;D1;+0:9])-[C:7]1-[C:6]-[#8:5]-[C:4]-[#7:3]-1-[C:2]=[O;D1;H0:1]
null
[]
null
null
1.5
HOUR
A solution of 9a (108 mg, 0.44 mmol) in ether (1 mL) is added dropwise to a cold (5°) solution of EtMgBr (3M in ether, 0.36 mL). The cold bath is removed, a crystal of iodine is added to the mixture and stirring is continued for 1.5 h at room temperature. The resulting mixture is diluted with EtOAc and washed with satu...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Secondary alcohol
null
null
C1COC[NH]1
Other
CCOCC
null
1.5
CCCCCCC(=O)N1[C@H](C=O)COC1(C)C>CCOCC>CCCCCCC(=O)N1[C@H](C(O)CC)COC1(C)C
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-160aa4a07a0a4c1883d138198c5f37bd
CC(C)(C)[Si](C)(C)Cl.CCCCCCC(=O)NC(CO)C(C)O>>CCCCCCC(=O)NC(CO[Si](C)(C)C(C)(C)C)C(C)O
OC(C(CO)NC(CCCCCC)=O)C.[Si](C)(C)(C(C)(C)C)Cl.C(C)N(CC)CC>>CC(C)(C)[Si](OCC(C(C)O)NC(CCCCCC)=O)(C)C
Cl[Si:13]([CH3:14])([CH3:15])[C:16]([CH3:17])([CH3:18])[CH3:19].[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[NH:9][CH:10]([CH2:11][OH:12])[CH:20]([CH3:21])[OH:22]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[NH:9][CH:10]([CH2:11][O:12][Si:13]([CH3:14])([CH3:15])[C:16]([CH3:17])([CH3:18])[CH3:19])...
CC(C)(C)[Si](C)(C)Cl.CCCCCCC(=O)NC(CO)C(C)O
CCCCCCC(=O)NC(CO[Si](C)(C)C(C)(C)C)C(C)O
null
CN(C1=CC=NC=C1)C
O.C(Cl)Cl
Protection
Alcohol protection with silyl ethers
0085cd6629412592263fdf1537bdf8c19ef10dbeafe6f880807464d8107fa715
d2a170d01b2f3ec57d6fac058519475050ba5531f5d304635fb42e153d5bb9b5
null
Cl-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7].[C:8]-[C:9]-[OH;D1;+0:10]>>[C:8]-[C:9]-[O;H0;D2;+0:10]-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7]
109.5
[{"value": 109.5, "product": "CC(C)(C)[Si](OCC(C(C)O)NC(CCCCCC)=O)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A mixture of 11c, (1.945 g) of t-butyldimethylsilyl chloride, (1.4165 g) of triethylamine (951 mg, 1.31 mL), and 4-dimethylaminopyridine (42.76 mg) in 13 mL of methylene chloride is stirred under argon at room temperature for 18 h. The reaction mixture is diluted with methylene chloride and water added. The organic lay...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Silyl protective group
TMS ether protective group
null
null
null
HCl
CN(C1=CC=NC=C1)C.O.C(Cl)Cl
null
18
CC(C)(C)[Si](C)(C)Cl.CCCCCCC(=O)NC(CO)C(C)O>CN(C1=CC=NC=C1)C.O.C(Cl)Cl>CCCCCCC(=O)NC(CO[Si](C)(C)C(C)(C)C)C(C)O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-2ac639f6a6d7446bbbb8b363582dbac2
CCCCCCC(=O)NC(CO[Si](C)(C)C(C)(C)C)C(C)O>>CCCCCCC(=O)N[C@@H](CO[Si](C)(C)C(C)(C)C)C(C)=O
CC(C)(C)[Si](OCC(C(C)O)NC(CCCCCC)=O)(C)C.[Cr](=O)(=O)([O-])O[Cr](=O)(=O)[O-].[NH+]1=CC=CC=C1.[NH+]1=CC=CC=C1>>CC(C)(C)[Si](OC[C@@H](C(C)=O)NC(CCCCCC)=O)(C)C
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[NH:9][CH:10]([CH2:11][O:12][Si:13]([CH3:14])([CH3:15])[C:16]([CH3:17])([CH3:18])[CH3:19])[CH:20]([CH3:21])[OH:22]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7](=[O:8])[NH:9][C@@H:10]([CH2:11][O:12][Si:13]([CH3:14])([CH3:15])[C:16]([CH3:17])([CH3:18])[CH3:19])[C...
CCCCCCC(=O)NC(CO[Si](C)(C)C(C)(C)C)C(C)O
CCCCCCC(=O)N[C@@H](CO[Si](C)(C)C(C)(C)C)C(C)=O
null
null
O.CN(C=O)C
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
c7c20d2959ac48847b03cc1265962cf99a8ec8a85900c087dabb30077298c66c
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
null
[#8:1]-[C:2]-[CH;D3;+0:3](-[#7:4]-[C:5](-[C:6])=[O;D1;H0:7])-[CH;D3;+0:8](-[C;D1;H3:9])-[OH;D1;+0:10]>>[#8:1]-[C:2]-[C@H;D3;+0:3](-[#7:4]-[C:5](-[C:6])=[O;D1;H0:7])-[C;H0;D3;+0:8](-[C;D1;H3:9])=[O;H0;D1;+0:10]
81.8
[{"value": 81.8, "product": "CC(C)(C)[Si](OC[C@@H](C(C)=O)NC(CCCCCC)=O)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A mixture of (10c), (2.30 g, 6.94 mmol) and pyridinium dichromate (10.62 g, 28.2 mmol) in 20 mL of N,N-dimethylformamide is stirred under argon for 18 h. The reaction mixture is diluted with 100 mL of water and extracted with ethyl acetate (3×40 mL). The organic layer is separated, washed with water and brine, dried an...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
null
null
null
null
O.CN(C=O)C
null
18
CCCCCCC(=O)NC(CO[Si](C)(C)C(C)(C)C)C(C)O>O.CN(C=O)C>CCCCCCC(=O)N[C@@H](CO[Si](C)(C)C(C)(C)C)C(C)=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-679238dd29464869b20e3dd2c6f6680b
O=C(O)CC[C@H]1C(=O)OCN1C(=O)OCc1ccccc1>>O=CCC[C@H]1C(=O)OCN1C(=O)OCc1ccccc1
O=C1[C@@H](N(CO1)C(=O)OCC1=CC=CC=C1)CCC(=O)O.[Cr](=O)(=O)([O-])Cl.[NH+]1=CC=CC=C1>>O=C1[C@@H](N(CO1)C(=O)OCC1=CC=CC=C1)CCC=O
O[C:2](=[O:1])[CH2:3][CH2:4][C@H:5]1[C:6](=[O:7])[O:8][CH2:9][N:10]1[C:11](=[O:12])[O:13][CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1>>[O:1]=[CH:2][CH2:3][CH2:4][C@H:5]1[C:6](=[O:7])[O:8][CH2:9][N:10]1[C:11](=[O:12])[O:13][CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1
O=C(O)CC[C@H]1C(=O)OCN1C(=O)OCc1ccccc1
O=CCC[C@H]1C(=O)OCN1C(=O)OCc1ccccc1
null
null
C(Cl)Cl.C1CCOC1
Reduction
OtherReaction
78999da0d33b2c10ff8c3d41626c41ea14d2697ff6d1d7e5baf78453ec38592a
f41d7c101137b93550fdf296ceb4547d1ce640e4cbceb5b7b006723d153456c9
O=C1CN(C(=O)OCc2ccccc2)CO1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]>>[C:4]-[C:3]-[CH;D2;+0:1]=[O;D1;H0:2]
51.4
[{"value": 51.4, "product": "O=C1[C@@H](N(CO1)C(=O)OCC1=CC=CC=C1)CCC=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
12
HOUR
A solution of 27 g (92.7 mmol) of the crude acid (43c) in 200 mL of THF is cooled to 0° C. and 13 mL (10.7 g, 141 mmol) of borane-methyl sulfide complex is added dropwise via an addition funnel. The reaction is allowed to warm gradually to room temperature and stirred for 12 h. The resulting mixture is concentrated in ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Aldehyde
null
null
C1COC[NH]1.c1ccccc1
Other
C(Cl)Cl.C1CCOC1
null
12
O=C(O)CC[C@H]1C(=O)OCN1C(=O)OCc1ccccc1>C(Cl)Cl.C1CCOC1>O=CCC[C@H]1C(=O)OCN1C(=O)OCc1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-26d5c56c33f14a27bcfc5293e42d4237
COC(=O)C(=CCCC1C(=O)OCN1C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C.COC(=O)[C@@H](C)N>>COC(=O)/C(=C/CC[C@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C
COC([C@H](N)C)=O.C1(=CC=CC=C1)COC(=O)N1COC(C1CCC=C(C(=O)OC)NC(=O)OC(C)(C)C)=O.COC([C@H](N)C)=O>>COC([C@H](NC([C@@H](NC(=O)OCC1=CC=CC=C1)CC\C=C(/NC(=O)OC(C)(C)C)\C(=O)OC)=O)C)=O
C1O[C:21](=[O:22])[CH:9]([CH2:8][CH2:7][CH:6]=[C:5]([C:3]([O:2][CH3:1])=[O:4])[NH:30][C:31](=[O:32])[O:33][C:34]([CH3:35])([CH3:36])[CH3:37])[N:10]1[C:11](=[O:12])[O:13][CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1.[NH2:23][C@H:24]([CH3:25])[C:26](=[O:27])[O:28][CH3:29]>>[CH3:1][O:2][C:3](=[O:4])/[C:5](=[CH:6]/[C...
COC(=O)C(=CCCC1C(=O)OCN1C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C.COC(=O)[C@@H](C)N
COC(=O)/C(=C/CC[C@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C
null
null
null
Protection
Displacement of ethoxy group by primary amine
e66d38b79edbc67df95fcb4abe49f899502b76bda3019f3ed03a0713db3334de
ea4684e285b3bc93becd6db94f29982da7cfdb0828955af8ce9c5dd9c972430f
c1ccccc1
[C;D1;H3:1]-[C:2](-[NH2;D1;+0:3])-[C:4](=[O;D1;H0:5])-[#8:6]-[C;D1;H3:7].[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[N;H0;D3;+0:12]1-C-O-[C;H0;D3;+0:13](=[O;D1;H0:14])-[CH;D3;+0:15]-1-[C:16]-[C:17]-[C:18]=[C:19]>>[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[NH;D2;+0:12]-[C@@H;D3;+0:15](-[C:16]-[C:17]/[C:18]=[C:19])-[C;H0;D3;+0:13](=[O;...
70.2
[{"value": 70.2, "product": "COC([C@H](NC([C@@H](NC(=O)OCC1=CC=CC=C1)CC\\C=C(/NC(=O)OC(C)(C)C)\\C(=O)OC)=O)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
140
CELSIUS
10
MINUTE
A mixture of 3.3 g of D-alanine methyl ester and 7.1 g of 46c is heated at 140° C. for 10 min, then another 1.6 g of D-alanine methyl ester is added. Heating is continued at 140° C. for an additional 10 min. After cooling to ambient temperature the crude product is chromatographed on silica gel using variable gradient ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ester.Primary amine
Carbamic ester.Secondary amide
C1COC[NH]1
null
c1ccccc1
HO-
null
140
0.166667
COC(=O)C(=CCCC1C(=O)OCN1C(=O)OCc1ccccc1)NC(=O)OC(C)(C)C.COC(=O)[C@@H](C)N>>COC(=O)/C(=C/CC[C@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-c10aac4f4a5d462eb61c169d6e23c1c5
COC(=O)/C(=C/CC[C@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C>>COC(=O)C(CCC[C@@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C
COC([C@H](NC([C@@H](NC(=O)OCC1=CC=CC=C1)CC\C=C(/NC(=O)OC(C)(C)C)\C(=O)OC)=O)C)=O.[H][H]>>COC([C@H](NC([C@H](NC(=O)OCC1=CC=CC=C1)CCCC(NC(=O)OC(C)(C)C)C(=O)OC)=O)C)=O
[CH3:1][O:2][C:3](=[O:4])/[C:5](=[CH:6]/[CH2:7][CH2:8][C@H:9]([NH:10][C:11](=[O:12])[O:13][CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1)[C:21](=[O:22])[NH:23][C@H:24]([CH3:25])[C:26](=[O:27])[O:28][CH3:29])[NH:30][C:31](=[O:32])[O:33][C:34]([CH3:35])([CH3:36])[CH3:37]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][CH2:...
COC(=O)/C(=C/CC[C@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C
COC(=O)C(CCC[C@@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C
null
Cl(=O)(=O)(=O)[O-].[Rh+]
C(C)(=O)O.C1CCOC1
Reduction
Hydrogenation (double to single)
c5482e96d32f880dae9cdf88ceb576b12289d0a709a9745c321f8f5233d183f3
b586296faf9080b398947dcba4825d3daf71a75997a309df19187f20bff3e49d
c1ccccc1
[C:1]-[C:2]/[CH;D2;+0:3]=[C;H0;D3;+0:4](\[#7:5]-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12])-[C:13](=[O;D1;H0:14])-[#8:15]-[C;D1;H3:16]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[CH;D3;+0:4](-[#7:5]-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12])-[C:13](=[O;D1;H0:14])-[#8:1...
92.6
[{"value": 92.6, "product": "COC([C@H](NC([C@H](NC(=O)OCC1=CC=CC=C1)CCCC(NC(=O)OC(C)(C)C)C(=O)OC)=O)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 8.5 g of 47c in 25 mL of acetic acid and 250 mL of THF is hydrogenated at 48 psi of hydrogen over 0.5 g of (bicyclo(2.2.1.)hepta-2,5-diene[2S,3S]bis(diphenylphosphino)butane)rhodium(I) perchlorate for 18 h. The reaction is filtered and evaporated to a residue. The residue is chromatographed using variable...
10.6084/m9.figshare.5104873.v1
null
Enamine
Ester
null
null
c1ccccc1
null
Cl(=O)(=O)(=O)[O-].[Rh+].C(C)(=O)O.C1CCOC1
null
null
COC(=O)/C(=C/CC[C@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C>Cl(=O)(=O)(=O)[O-].[Rh+].C(C)(=O)O.C1CCOC1>COC(=O)C(CCC[C@@H](NC(=O)OCc1ccccc1)C(=O)N[C@H](C)C(=O)OC)NC(=O)OC(C)(C)C
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-fe2f4f1f21b644dbbc12c75cafdad403
CCCCCCC(=O)NC(CNC(=O)N[C@@H](CCCC(NC(=O)OC(C)(C)C)C(=O)O)C(=O)N[C@H](C)C(=O)O)C(=O)O>>CCCCCCC(=O)NC(CNC(=O)N[C@@H](CCCC(N)C(=O)O)C(=O)N[C@H](C)C(=O)O)C(=O)O
C(=O)(O)C(CCC[C@H](NC(=O)NCC(NC(CCCCCC)=O)C(=O)O)C(=O)N[C@H](C)C(=O)O)NC(=O)OC(C)(C)C>>C(=O)(O)C(CCC[C@H](NC(=O)NCC(NC(CCCCCC)=O)C(=O)O)C(=O)N[C@H](C)C(=O)O)N
CC(C)(C)OC(=O)[NH:21][CH:20]([CH2:19][CH2:18][CH2:17][C@H:16]([NH:15][C:13]([NH:12][CH2:11][CH:10]([NH:9][C:7]([CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])=[O:8])[C:33](=[O:34])[OH:35])=[O:14])[C:25](=[O:26])[NH:27][C@H:28]([CH3:29])[C:30](=[O:31])[OH:32])[C:22](=[O:23])[OH:24]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6...
CCCCCCC(=O)NC(CNC(=O)N[C@@H](CCCC(NC(=O)OC(C)(C)C)C(=O)O)C(=O)N[C@H](C)C(=O)O)C(=O)O
CCCCCCC(=O)NC(CNC(=O)N[C@@H](CCCC(N)C(=O)O)C(=O)N[C@H](C)C(=O)O)C(=O)O
null
null
C(=O)(C(F)(F)F)O
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
null
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4](=[O;D1;H0:5])-[O;D1;H1:6]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4](=[O;D1;H0:5])-[O;D1;H1:6]
null
[]
null
null
null
null
To 85.9 mg of 1b-5 under argon is treated with 500 μl of TFA according to Example 80. The volatiles are evaporated to a residue which is triturated with ether 3× and the ether is decanted. The residue is dried to give 77.9 mg of 1b-11 as a white solid. NMR (CD3OD) δ 0.80 (t, 3 H), 2.16 (t, 2 H), 3.22 (br s, 5 H), 3.58 ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
null
HO-
C(=O)(C(F)(F)F)O
null
null
CCCCCCC(=O)NC(CNC(=O)N[C@@H](CCCC(NC(=O)OC(C)(C)C)C(=O)O)C(=O)N[C@H](C)C(=O)O)C(=O)O>C(=O)(C(F)(F)F)O>CCCCCCC(=O)NC(CNC(=O)N[C@@H](CCCC(N)C(=O)O)C(=O)N[C@H](C)C(=O)O)C(=O)O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-f65db27a2d674478893e33364067f34e
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2sc([N+](=O)[O-])cc21>>O=C1CC2(CCNCC2)Sc2sc([N+](=O)[O-])cc21
[N+](=O)([O-])C1=CC2=C(SC3(CC2=O)CCN(CC3)C(C3=CC=CC=C3)=O)S1.Cl>>Cl.[N+](=O)([O-])C1=CC2=C(SC3(CC2=O)CCNCC3)S1
O=C(c1ccccc1)[N:8]1[CH2:7][CH2:6][C:5]2([CH2:4][C:3](=[O:2])[c:19]3[c:12]([s:13][c:14]([N+:15](=[O:16])[O-:17])[cH:18]3)[S:11]2)[CH2:10][CH2:9]1>>[O:2]=[C:3]1[CH2:4][C:5]2([CH2:6][CH2:7][NH:8][CH2:9][CH2:10]2)[S:11][c:12]2[s:13][c:14]([N+:15](=[O:16])[O-:17])[cH:18][c:19]21
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2sc([N+](=O)[O-])cc21
O=C1CC2(CCNCC2)Sc2sc([N+](=O)[O-])cc21
null
null
CO
Reduction
Hydrogenolysis of tertiary amines
061972243e5df2c50b2abe297b51515d793d6e04c114daffd44fd3c09d1f35a1
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
O=C1CC2(CCNCC2)Sc2sccc21
O=C(-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5])-c1:c:c:c:c:c:1>>[C:5]-[C:4]-[NH;D2;+0:1]-[C:2]-[C:3]
73
[{"value": 73.0, "product": "Cl.[N+](=O)([O-])C1=CC2=C(SC3(CC2=O)CCNCC3)S1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A suspension of 1.1 g (2.9 mmol) Of 2'-nitro-1-(benzoyl)spiro(piperidine-4,6'-(6H)thieno[2,3-b]thiopyran)-4'(5'H)-one in 25 mL methanol was treated with 25 ml of 6N HCl and heated to reflux for 3 days. The reaction was cooled to ambient temperature and the solid collected and dried in vacuo, to give 680 mg (73%) of the...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccccc1.c1cc2c(s1)SC1(CC[NH]CC1)CC2
c1cc2c(s1)SC1(CCNCC1)CC2
c1cc2c(s1)SC1(CCNCC1)CC2
HO-
CO
null
null
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2sc([N+](=O)[O-])cc21>CO>O=C1CC2(CCNCC2)Sc2sc([N+](=O)[O-])cc21
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ec57176989cf4ac985f33c1e593bb213
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2sccc21>>O=C1CC2(CCNCC2)Sc2sccc21
C(C1=CC=CC=C1)(=O)N1CCC2(CC(C3=C(S2)SC=C3)=O)CC1.Cl>>Cl.S1C=CC2=C1SC1(CC2=O)CCNCC1
O=C(c1ccccc1)[N:8]1[CH2:7][CH2:6][C:5]2([CH2:4][C:3](=[O:2])[c:16]3[c:12]([s:13][cH:14][cH:15]3)[S:11]2)[CH2:10][CH2:9]1>>[O:2]=[C:3]1[CH2:4][C:5]2([CH2:6][CH2:7][NH:8][CH2:9][CH2:10]2)[S:11][c:12]2[s:13][cH:14][cH:15][c:16]21
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2sccc21
O=C1CC2(CCNCC2)Sc2sccc21
null
null
C(C)O
Reduction
Hydrogenolysis of tertiary amines
061972243e5df2c50b2abe297b51515d793d6e04c114daffd44fd3c09d1f35a1
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
O=C1CC2(CCNCC2)Sc2sccc21
O=C(-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5])-c1:c:c:c:c:c:1>>[C:5]-[C:4]-[NH;D2;+0:1]-[C:2]-[C:3]
null
[]
null
null
null
null
A solution of 14 g (40.99 mmol) of 1-benzoylspiro(piperidine-4,6'-(6H)thieno[2,3-b]thiopyran)-4'-(5'H)-one in 150 ml of ethanol was treated with 50 ml of 6N HCl and heated at reflux for 2 days. The reaction was cooled to room temperature and the solid collected by filtration. The solid was dried overnight in vacuo to g...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccccc1.c1cc2c(s1)SC1(CC[NH]CC1)CC2
c1cc2c(s1)SC1(CCNCC1)CC2
c1cc2c(s1)SC1(CCNCC1)CC2
HO-
C(C)O
null
null
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2sccc21>C(C)O>O=C1CC2(CCNCC2)Sc2sccc21
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ed27f126b77d43e6a1c1da3462a9297f
Cl.O=C1CC2(CCN(CCc3ccc([N+](=O)[O-])cc3)CC2)Sc2sccc21>>Cl.Cl.Cl.Nc1ccc(CCN2CCC3(CC2)CC(=O)c2ccsc2S3)cc1.Nc1ccc(CCN2CCC3(CC2)CC(=O)c2ccsc2S3)cc1.O
[OH-].[Na+].Cl.[N+](=O)([O-])C1=CC=C(C=C1)CCN1CCC2(CC(C3=C(S2)SC=C3)=O)CC1.Cl.C([O-])(O)=O.[Na+]>>O.Cl.Cl.NC1=CC=C(C=C1)CCN1CCC2(CC(C3=C(S2)SC=C3)=O)CC1.NC1=CC=C(C=C1)CCN1CCC3(CC(C2=C(S3)SC=C2)=O)CC1.Cl.Cl
[ClH:4].[O-][N+:5]([c:6]1[cH:28][cH:32][c:33]([CH2:34][CH2:35][N:36]2[CH2:7][CH2:14][C:15]3([CH2:18][C:19](=[O:20])[c:21]4[cH:22][cH:47][s:48][c:25]4[S:24]3)[CH2:38][CH2:37]2)[cH:51][cH:52]1)=[O:53]>>[ClH:2].[ClH:3].[ClH:4].[NH2:5][c:6]1[cH:7][cH:8][c:9]([CH2:10][CH2:11][N:12]2[CH2:13][CH2:14][C:15]3([CH2:16][CH2:17]2)...
Cl.O=C1CC2(CCN(CCc3ccc([N+](=O)[O-])cc3)CC2)Sc2sccc21
Cl.Cl.Cl.Nc1ccc(CCN2CCC3(CC2)CC(=O)c2ccsc2S3)cc1.Nc1ccc(CCN2CCC3(CC2)CC(=O)c2ccsc2S3)cc1.O
null
null
O.C(C)(=O)O
Aromatic Heterocycle Formation
OtherReaction
c56dd5904255ec4f258ab23d7047a9b77ea93071792ad667135d8c6cd39478ca
2bf816a2e72d2b6a7215a1d0134bbb0cd11b5ceb8cd441ecbc869f832ce16ff5
O=C1CC2(CCN(CCc3ccccc3)CC2)Sc2sccc21.O=C1CC2(CCN(CCc3ccccc3)CC2)Sc2sccc21
[O-]-[N+;H0;D3:1](=[O;H0;D1;+0:2])-[c;H0;D3;+0:3]1:[cH;D2;+0:4]:[cH;D2;+0:5]:[c:6](-[C:7]-[C:8]-[N;H0;D3;+0:9]2-[C:10]-[CH2;D2;+0:11]-[C;H0;D4;+0:12]3(-[C:13]-[C:14](=[O;D1;H0:15])-[c:16]4:[cH;D2;+0:17]:[cH;D2;+0:18]:[s;H0;D2;+0:19]:[c;H0;D3;+0:20]:4-[S;H0;D2;+0:21]-3)-[CH2;D2;+0:22]-[CH2;D2;+0:23]-2):[c:24]:[cH;D2;+0:...
null
[]
null
null
45
MINUTE
A solution Of 1.1 g (2.8 mmoles) of 1-(2-(p-nitrophenyl)ethyl)spiro(piperidine-4,6'-(6H)-thieno-[2,3-b]thiopyran)-4'(5'H)-one in 15 mL acetic acid and 20 mL H2O was treated with 15 mL of a solution of 15% TiCl3 in 20% HCl. The dark purple reaction mixture was stirred at room temperature for 45 minutes and poured into 2...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Tertiary amine.Monosulfide
Ketone.Primary amine.Primary amine.Tertiary amine.Tertiary amine.Monosulfide.Monosulfide
c1ccccc1.c1cc2c(s1)SC1(CC[NH]CC1)CC2
c1ccccc1.c1cc2c(s1)SC1(CC[NH]CC1)CC2.c1ccccc1.c1cc2c(s1)SC1(CC[NH]CC1)CC2
c1ccccc1.c1cc2c(s1)SC1(CC[NH]CC1)CC2.c1ccccc1.c1cc2c(s1)SC1(CC[NH]CC1)CC2
null
O.C(C)(=O)O
null
0.75
Cl.O=C1CC2(CCN(CCc3ccc([N+](=O)[O-])cc3)CC2)Sc2sccc21>O.C(C)(=O)O>Cl.Cl.Cl.Nc1ccc(CCN2CCC3(CC2)CC(=O)c2ccsc2S3)cc1.Nc1ccc(CCN2CCC3(CC2)CC(=O)c2ccsc2S3)cc1.O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-2436bfb999cc4109bb710634b257b137
BrCc1ccccc1.CCOC(=O)C1CCN(C(=O)c2ccccc2)CC1>>CCOC(=O)C1(Cc2ccccc2)CCN(C(=O)c2ccccc2)CC1
C(C1=CC=CC=C1)Br.C[Si](C)(C)[N-][Si](C)(C)C.[Li+].C(C1=CC=CC=C1)(=O)N1CCC(CC1)C(=O)OCC>>C(C)OC(=O)C1(CCN(CC1)C(C1=CC=CC=C1)=O)CC1=CC=CC=C1
Br[CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1.[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]1[CH2:14][CH2:15][N:16]([C:17](=[O:18])[c:19]2[cH:20][cH:21][cH:22][cH:23][cH:24]2)[CH2:25][CH2:26]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]1([CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[CH2:14][CH2:15][N:16]([C:17](=[O:18])[c:...
BrCc1ccccc1.CCOC(=O)C1CCN(C(=O)c2ccccc2)CC1
CCOC(=O)C1(Cc2ccccc2)CCN(C(=O)c2ccccc2)CC1
null
null
O1CCCC1
C-C Coupling
OtherReaction
cc17dfd0def644ca87e815e637357310f207eb90d8b3273b51858e3602d79eca
0061a06af9fc64155952582b91b574e4abd8908ca14244f15179c2400b24dd08
O=C(c1ccccc1)N1CCC(Cc2ccccc2)CC1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[CH;D3;+0:9]1-[C:10]-[C:11]-[#7:12]-[C:13]-[C:14]-1>>[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[C;H0;D4;+0:9]1(-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10]-[C:11]-[#7:12]-[C:13]-[C:14]-1
118.6
[{"value": 118.6, "product": "C(C)OC(=O)C1(CCN(CC1)C(C1=CC=CC=C1)=O)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 7.84 g (30.0 mmoles) ethyl 1-benzoyl-4-piperidinecarboxylate (G. R. Clemo and E. Hoggarth, J. Chem. Soc., 41, (1941) in 60 ml dry. tetrahydrofuran at -78° C. under argon was added dropwise over 10 minutes 33.0 ml (33.0 mmoles) lithium bis(trimethylsilyl)amide in tetrahydrofuran and the resulting soluti...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester
Ester
C1CC[NH]CC1
C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1.c1ccccc1
HBr
O1CCCC1
null
0.5
BrCc1ccccc1.CCOC(=O)C1CCN(C(=O)c2ccccc2)CC1>O1CCCC1>CCOC(=O)C1(Cc2ccccc2)CCN(C(=O)c2ccccc2)CC1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-503ce7328877430c83c2dad8690e18c2
CCOC(=O)C1(Cc2ccccc2)CCN(C(=O)c2ccccc2)CC1>>O=C(c1ccccc1)N1CCC(Cc2ccccc2)(C(=O)O)CC1
Cl.C(C1=CC=CC=C1)(=O)N1CCC(CC1)(C(=O)OCC)CC1=CC=CC=C1.CC(C)([O-])C.[K+]>>C(C1=CC=CC=C1)(=O)N1CCC(CC1)(C(=O)O)CC1=CC=CC=C1
CC[O:22][C:20]([C:12]1([CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][cH:19]2)[CH2:11][CH2:10][N:9]([C:2](=[O:1])[c:3]2[cH:4][cH:5][cH:6][cH:7][cH:8]2)[CH2:24][CH2:23]1)=[O:21]>>[O:1]=[C:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1)[N:9]1[CH2:10][CH2:11][C:12]([CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][cH:19]2)([C:20](=[O:21...
CCOC(=O)C1(Cc2ccccc2)CCN(C(=O)c2ccccc2)CC1
O=C(c1ccccc1)N1CCC(Cc2ccccc2)(C(=O)O)CC1
null
null
CS(=O)C
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C(c1ccccc1)N1CCC(Cc2ccccc2)CC1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
78.9
[{"value": 75.0, "product": "C(C1=CC=CC=C1)(=O)N1CCC(CC1)(C(=O)O)CC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.9, "product": "C(C1=CC=CC=C1)(=O)N1CCC(CC1)(C(=O)O)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To 10.7 g (26 mmoles) crude ethyl 1-benzoyl-4-(phenylmethyl)-4-piperidinecarboxylate was added a solution of 14.6 g (130 mmoles) potassium tert-butoxide in 130 ml dimethyl sulfoxide. The resulting purple solution was stirred 2 hours to give a dark orange solution. The solution was poured into 500 ml rapidly stirred ice...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.C1CC[NH]CC1.c1ccccc1
Other
CS(=O)C
null
2
CCOC(=O)C1(Cc2ccccc2)CCN(C(=O)c2ccccc2)CC1>CS(=O)C>O=C(c1ccccc1)N1CCC(Cc2ccccc2)(C(=O)O)CC1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-912fda52d8fa431a8028fa3907b7ca92
O=C(c1ccccc1)N1CCC(Cc2ccccc2)(C(=O)O)CC1>>O=C(c1ccccc1)N1CCC2(CC1)Cc1ccccc1C2=O
C(C1=CC=CC=C1)(=O)N1CCC(CC1)(C(=O)O)CC1=CC=CC=C1>>C(C1=CC=CC=C1)(=O)N1CCC2(CC1)C(C1=CC=CC=C1C2)=O
O[C:22]([C:12]1([CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:11][CH2:10][N:9]([C:2](=[O:1])[c:3]2[cH:4][cH:5][cH:6][cH:7][cH:8]2)[CH2:14][CH2:13]1)=[O:23]>>[O:1]=[C:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1)[N:9]1[CH2:10][CH2:11][C:12]2([CH2:13][CH2:14]1)[CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][c:21]1[C:2...
O=C(c1ccccc1)N1CCC(Cc2ccccc2)(C(=O)O)CC1
O=C(c1ccccc1)N1CCC2(CC1)Cc1ccccc1C2=O
null
null
O
Functional Group Interconversion
OtherReaction
787ba820e569522607c2c82759edd12708de635414a7ad7ece07bc54eae6a030
6a71bb5a71b59feeb4f6a39b1b66fa450a058b64b0a3909e1a51c22473a141c5
O=C(c1ccccc1)N1CCC2(CC1)Cc1ccccc1C2=O
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4]-[c:5](:[c:6]):[cH;D2;+0:7]:[c:8]:[c:9])(-[C:10])-[C:11]>>[C:10]-[C:3]1(-[C:11])-[C:4]-[c:5](:[c:6]):[c;H0;D3;+0:7](:[c:8]:[c:9])-[C;H0;D3;+0:1]-1=[O;D1;H0:2]
62.2
[{"value": 62.0, "product": "C(C1=CC=CC=C1)(=O)N1CCC2(CC1)C(C1=CC=CC=C1C2)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.2, "product": "C(C1=CC=CC=C1)(=O)N1CCC2(CC1)C(C1=CC=CC=C1C2)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of 6.14 g (19.0 mmoles) 1-benzoyl-4-(phenylmethyl)-4-piperidinecarboxylic acid in 61 ml concentrated sulfuzic acid was stirred 18 hours at room temperature to give a deep red solution. The solution was carefully diluted with ice-bath cooling with 300 ml H2O and extracted with 3×300 ml ethyl acetate. The extr...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ketone
c1ccccc1
c1ccc2c(c1)CC1(CC[NH]CC1)C2
c1ccccc1.c1ccc2c(c1)CC1(CC[NH]CC1)C2
HO-
O
null
18
O=C(c1ccccc1)N1CCC(Cc2ccccc2)(C(=O)O)CC1>O>O=C(c1ccccc1)N1CCC2(CC1)Cc1ccccc1C2=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-81b58828189c480a90bc85d00cc71504
O=C(c1ccccc1)N1CCC2(CC1)Cc1ccccc1C2=O>>O=C1c2ccccc2CC12CCNCC2
C(C1=CC=CC=C1)(=O)N1CCC2(CC1)C(C1=CC=CC=C1C2)=O>>O=C1C2=CC=CC=C2CC12CCNCC2
O=C(c1ccccc1)[N:13]1[CH2:12][CH2:11][C:10]2([C:2](=[O:1])[c:3]3[cH:4][cH:5][cH:6][cH:7][c:8]3[CH2:9]2)[CH2:15][CH2:14]1>>[O:1]=[C:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][C:10]12[CH2:11][CH2:12][NH:13][CH2:14][CH2:15]2
O=C(c1ccccc1)N1CCC2(CC1)Cc1ccccc1C2=O
O=C1c2ccccc2CC12CCNCC2
null
null
Cl.C(C)O
Reduction
Hydrogenolysis of tertiary amines
20ff99edc06d17eb1c5ccc5ceb37a19d52a788336a8df7f05fa1526dc6598528
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
O=C1c2ccccc2CC12CCNCC2
O=C(-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5])-c1:c:c:c:c:c:1>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
77.4
[{"value": 77.0, "product": "O=C1C2=CC=CC=C2CC12CCNCC2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.4, "product": "O=C1C2=CC=CC=C2CC12CCNCC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3.66 g (12.0 mmoles) 1'-benzoyl-1,3-dihydro-1-oxospiro-[2H-indene-2,4'-piperidine] in 90 ml ethanol and 30 ml 6N hydrochloric acid was heated at reflux for 42 hours. An additional 10 ml 6N hydrochloric acid was added and the solution was heated at reflux for 6 hours. The cooled solution was concentrated i...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccccc1.c1ccc2c(c1)CC1(CC[NH]CC1)C2
c1ccc2c(c1)CC1(CCNCC1)C2
c1ccc2c(c1)CC1(CCNCC1)C2
HO-
Cl.C(C)O
null
null
O=C(c1ccccc1)N1CCC2(CC1)Cc1ccccc1C2=O>Cl.C(C)O>O=C1c2ccccc2CC12CCNCC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-605cac8cff47459890dbd04581014144
O=C1c2ccccc2CC12CCNCC2.O=[N+]([O-])c1ccc(CCBr)cc1>>O=C1c2ccccc2CC12CCN(CCc1ccc([N+](=O)[O-])cc1)CC2
O=C1C2=CC=CC=C2CC12CCNCC2.[N+](=O)([O-])C1=CC=C(CCBr)C=C1.C([O-])(O)=O.[Na+]>>O=C1C2=CC=CC=C2CC12CCN(CC2)CCC2=CC=C(C=C2)[N+](=O)[O-]
[O:1]=[C:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][C:10]12[CH2:11][CH2:12][NH:13][CH2:25][CH2:26]2.Br[CH2:14][CH2:15][c:16]1[cH:17][cH:18][c:19]([N+:20](=[O:21])[O-:22])[cH:23][cH:24]1>>[O:1]=[C:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][C:10]12[CH2:11][CH2:12][N:13]([CH2:14][CH2:15][c:16]1[cH:17][cH:18][c:19]...
O=C1c2ccccc2CC12CCNCC2.O=[N+]([O-])c1ccc(CCBr)cc1
O=C1c2ccccc2CC12CCN(CCc1ccc([N+](=O)[O-])cc1)CC2
null
null
C(C)O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
b98f25b7f7ba26359793785ecff3964b918e34394e910ff6139ef5763b458f9f
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1c2ccccc2CC12CCN(CCc1ccccc1)CC2
Br-[CH2;D2;+0:1]-[C:2]-[c:3].[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8]>>[C:4]-[C:5]-[N;H0;D3;+0:6](-[CH2;D2;+0:1]-[C:2]-[c:3])-[C:7]-[C:8]
58
[{"value": 58.0, "product": "O=C1C2=CC=CC=C2CC12CCN(CC2)CCC2=CC=C(C=C2)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 56.2, "product": "O=C1C2=CC=CC=C2CC12CCN(CC2)CCC2=CC=C(C=C2)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 0.60 g (3.0 moles) 1,3-dihydro-1-oxospiro[2H-indene-2,4'-piperidine], 0.71 g (3.1 mmoles) 4-nitrophenethyl bromide, and 0.28 g (3.3 mmoles) sodium bicarbonate in 3 ml ethanol was heated at reflux for 6 hours. The solvent was removed in vacuo and the residue was partitioned between 20 ml ethyl acetate and 5...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
c1ccc2c(c1)CC1(CCNCC1)C2
c1ccc2c(c1)CC1(CC[NH]CC1)C2
c1ccc2c(c1)CC1(CC[NH]CC1)C2.c1ccccc1
HBr
C(C)O
null
null
O=C1c2ccccc2CC12CCNCC2.O=[N+]([O-])c1ccc(CCBr)cc1>C(C)O>O=C1c2ccccc2CC12CCN(CCc1ccc([N+](=O)[O-])cc1)CC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-5dfbaed87b85463b84e1def719b9b3e4
CC(=O)N1CCC2(CC1)Cc1ccc([N+](=O)[O-])cc1C2=O>>O=C1c2cc([N+](=O)[O-])ccc2CC12CCNCC2
C(C)(=O)N1CCC2(CC1)C(C1=CC(=CC=C1C2)[N+](=O)[O-])=O.Cl.Cl>>Cl.[N+](=O)([O-])C1=CC=C2CC3(CCNCC3)C(C2=C1)=O
CC(=O)[N:17]1[CH2:16][CH2:15][C:14]2([C:3](=[O:2])[c:4]3[cH:5][c:6]([N+:7](=[O:8])[O-:9])[cH:10][cH:11][c:12]3[CH2:13]2)[CH2:19][CH2:18]1>>[O:2]=[C:3]1[c:4]2[cH:5][c:6]([N+:7](=[O:8])[O-:9])[cH:10][cH:11][c:12]2[CH2:13][C:14]12[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]2
CC(=O)N1CCC2(CC1)Cc1ccc([N+](=O)[O-])cc1C2=O
O=C1c2cc([N+](=O)[O-])ccc2CC12CCNCC2
null
null
C(C)O
Reduction
Hydrogenolysis of tertiary amines
b1cb52270d580532affb153faf9496db8bc0156ff196af48791beb9b6968e4c4
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
O=C1c2ccccc2CC12CCNCC2
C-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
74.5
[{"value": 74.0, "product": "Cl.[N+](=O)([O-])C1=CC=C2CC3(CCNCC3)C(C2=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 74.5, "product": "Cl.[N+](=O)([O-])C1=CC=C2CC3(CCNCC3)C(C2=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 0.216 g (0.75 mmol) 1'-acetyl-1,3-dihydro-1-oxo-6-nitrospiro[2H-indene-2,4'-piperidine] and 2 ml (6 mmol) 3N hydrochloric acid in 6 ml ethanol was heated at reflux for 18 hours. Another 0.2 ml (0.6 mmol) 3N hydrochloric acid was added and the solution was heated at reflux for 4 hours, then cooled to room ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccc2c(c1)CC1(CC[NH]CC1)C2
c1ccc2c(c1)CC1(CCNCC1)C2
c1ccc2c(c1)CC1(CCNCC1)C2
HO-
C(C)O
null
null
CC(=O)N1CCC2(CC1)Cc1ccc([N+](=O)[O-])cc1C2=O>C(C)O>O=C1c2cc([N+](=O)[O-])ccc2CC12CCNCC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-55054c5686e74d75b17896bf1ce5c7ef
CC(=O)N1CCC2(CC1)Cc1ccc([N+](=O)[O-])cc1C2=O>>CC(=O)N1CCC2(CC1)Cc1ccc(N)cc1C2=O
C([O-])(O)=O.[Na+].C(C)(=O)N1CCC2(CC1)C(C1=CC(=CC=C1C2)[N+](=O)[O-])=O.[OH-].[Na+]>>C(C)(=O)N1CCC2(CC1)C(C1=CC(=CC=C1C2)N)=O
O=[N+:15]([O-])[c:14]1[cH:13][cH:12][c:11]2[c:17]([cH:16]1)[C:18](=[O:19])[C:7]1([CH2:6][CH2:5][N:4]([C:2]([CH3:1])=[O:3])[CH2:9][CH2:8]1)[CH2:10]2>>[CH3:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][C:7]2([CH2:8][CH2:9]1)[CH2:10][c:11]1[cH:12][cH:13][c:14]([NH2:15])[cH:16][c:17]1[C:18]2=[O:19]
CC(=O)N1CCC2(CC1)Cc1ccc([N+](=O)[O-])cc1C2=O
CC(=O)N1CCC2(CC1)Cc1ccc(N)cc1C2=O
null
[Cl-].[Ti+3].[Cl-].[Cl-]
Cl.O.C(C)(=O)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C1c2ccccc2CC12CCNCC2
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
112.3
[{"value": 112.3, "product": "C(C)(=O)N1CCC2(CC1)C(C1=CC(=CC=C1C2)N)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a solution of 0.29 g (1.0 mmole) 1'-acetyl-1,3-dihydro-6-nitro-1-oxospiro[2H-indene-2,4'-piperidine] in 4 ml acetic acid was added 3.75 ml (4.3 mmoles) of 15% titanium (III) chloride solution in 20-30% aqueous hydrochloric acid dropwise and portionwise over 2 hours. The reaction mixture was made basic (pH 10) with s...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2c(c1)CC1(CC[NH]CC1)C2
Other
[Cl-].[Ti+3].[Cl-].[Cl-].Cl.O.C(C)(=O)O
null
2
CC(=O)N1CCC2(CC1)Cc1ccc([N+](=O)[O-])cc1C2=O>[Cl-].[Ti+3].[Cl-].[Cl-].Cl.O.C(C)(=O)O>CC(=O)N1CCC2(CC1)Cc1ccc(N)cc1C2=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-35cf24df8bd9426d8ecf4c4423920048
CCOC(=O)N(CCBr)CCBr.O=C1CCCc2ccccc21>>CCOC(=O)N1CCC2(CCc3ccccc3C2=O)CC1
C1(CCCC2=CC=CC=C12)=O.BrCCN(C(OCC)=O)CCBr.[H-].[Na+]>>C(C)OC(=O)N1CCC2(CC1)C(C1=CC=CC=C1CC2)=O
Br[CH2:8][CH2:7][N:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:20][CH2:21]Br.[CH2:9]1[CH2:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[C:18]1=[O:19]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][C:9]2([CH2:10][CH2:11][c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[C:18]2=[O:19])[CH2:20][CH2:21]1
CCOC(=O)N(CCBr)CCBr.O=C1CCCc2ccccc21
CCOC(=O)N1CCC2(CCc3ccccc3C2=O)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
174cb1ade1a683a04eb358fc59febf7c715b90f9543d7ee4978ea7230242efd8
fc480cd11c4523824dc79fb530b6fe43274a09b2c3c6b9d6ec28ea3488f5f252
O=C1c2ccccc2CCC12CCNCC2
Br-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[N;H0;D3;+0:3](-[C:4]-[CH2;D2;+0:5]-Br)-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9].[C:10]-[C:11]-[CH2;D2;+0:12]-[C:13](=[O;D1;H0:14])-[c:15]>>[C:10]-[C:11]-[C;H0;D4;+0:12]1(-[CH2;D2;+0:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:3](-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9])-[C:4]-[CH2;D2;+0:5]-1)-[C:13](=[O;D1;H0:14])-[c...
26
[{"value": 26.0, "product": "C(C)OC(=O)N1CCC2(CC1)C(C1=CC=CC=C1CC2)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 25.6, "product": "C(C)OC(=O)N1CCC2(CC1)C(C1=CC=CC=C1CC2)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
14
HOUR
To a solution of 2.92 g (20.0 mmoles) 1-tetralone and 9.0 g (30.0 mmoles) ethyl bis(2-bromoethyl)carbamate (S. Huybuchts and G. J. Hoornaert, Synth. Commum., 11, 17 (1981) in 20 ml dry dimethylformamide heated to 50° C. under argon was added in portions 2.00 g (50.0 mmol) of 60% sodium hydride dispersion is mineral oil...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Carbamic ester.Ketone
Carbamic ester.Ketone
c1ccc2c(c1)CCCC2
c1ccc2c(c1)CCC1(CC[NH]CC1)C2
c1ccc2c(c1)CCC1(CC[NH]CC1)C2
HBr
CN(C=O)C
50
14
CCOC(=O)N(CCBr)CCBr.O=C1CCCc2ccccc21>CN(C=O)C>CCOC(=O)N1CCC2(CCc3ccccc3C2=O)CC1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-1235741b27ab474a8d96b42ef5a69254
CCN1CCC2(CCc3ccccc3C2=O)CC1>>O=C1c2ccccc2CCC12CCNCC2
C(C)N1CCC2(CC1)C(C1=CC=CC=C1CC2)=O>>O=C1C2=CC=CC=C2CCC12CCNCC2
CC[N:14]1[CH2:13][CH2:12][C:11]2([C:2](=[O:1])[c:3]3[cH:4][cH:5][cH:6][cH:7][c:8]3[CH2:9][CH2:10]2)[CH2:16][CH2:15]1>>[O:1]=[C:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][CH2:10][C:11]12[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]2
CCN1CCC2(CCc3ccccc3C2=O)CC1
O=C1c2ccccc2CCC12CCNCC2
null
null
[OH-].[K+].C(C)O
Deprotection
Hydrogenolysis of tertiary amines
57f31c421a16f46cceb8712fcca8a76ec9121c3c7e079834fb51cccafc97fdfe
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
O=C1c2ccccc2CCC12CCNCC2
C-C-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
78
[{"value": 78.0, "product": "O=C1C2=CC=CC=C2CCC12CCNCC2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.7, "product": "O=C1C2=CC=CC=C2CCC12CCNCC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 1.84 g (6.4 mmoles) ethyl 3,4-dihydro-1-oxospiro[naphthalene-2(1H),4'piperidine] in 32 ml ethanol and 16 ml of 50% potassium hydroxide solution was heated at reflux for 18 hours. The solution was concentrated in vacuo to remove ethanol and the aqueous residue was extracted with 3×40 ml ether. The combined...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccc2c(c1)CCC1(CC[NH]CC1)C2
c1ccc2c(c1)CCC1(CCNCC1)C2
c1ccc2c(c1)CCC1(CCNCC1)C2
Other
[OH-].[K+].C(C)O
null
null
CCN1CCC2(CCc3ccccc3C2=O)CC1>[OH-].[K+].C(C)O>O=C1c2ccccc2CCC12CCNCC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-76aa8d7938414f228e1d6142199342a2
CC(=O)N1CCC2(CCc3ccc(NS(C)(=O)=O)cc3C2=O)CC1>>CS(=O)(=O)Nc1ccc2c(c1)C(=O)C1(CCNCC1)CC2
Cl.C(C)(=O)N1CCC2(CC1)C(C1=CC(=CC=C1CC2)NS(=O)(=O)C)=O.Cl>>Cl.CS(=O)(=O)NC1=CC=C2CCC3(CCNCC3)C(C2=C1)=O
CC(=O)[N:17]1[CH2:16][CH2:15][C:14]2([C:12](=[O:13])[c:10]3[c:9]([cH:8][cH:7][c:6]([NH:5][S:2]([CH3:1])(=[O:3])=[O:4])[cH:11]3)[CH2:21][CH2:20]2)[CH2:19][CH2:18]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[C:12](=[O:13])[C:14]1([CH2:15][CH2:16][NH:17][CH2:18][CH2:19]1)[CH2:20][CH2:21]2
CC(=O)N1CCC2(CCc3ccc(NS(C)(=O)=O)cc3C2=O)CC1
CS(=O)(=O)Nc1ccc2c(c1)C(=O)C1(CCNCC1)CC2
null
null
C(C)O
Reduction
Hydrogenolysis of tertiary amines
9225235603486c1bf83e27f088d5a1b189d6acdd2949a4da12907d46f5e44d14
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
O=C1c2ccccc2CCC12CCNCC2
C-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
67
[{"value": 67.0, "product": "Cl.CS(=O)(=O)NC1=CC=C2CCC3(CCNCC3)C(C2=C1)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 0.53 g (1.5 mmoles) 1'-acetyl-3,4-dihydro-7-methanesulfonamido-1-oxospiro[naphthalene-2(1H),4'-piperidine] in 15 ml ethanol and 5 ml 3N hydrochloric acid was heated at reflux for 18 hours. An additional 10 ml 3N hydrochloric acid was added and the solution was heatea at reflux for 5 hours, then cooled to ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccc2c(c1)CCC1(CC[NH]CC1)C2
c1ccc2c(c1)CCC1(CCNCC1)C2
c1ccc2c(c1)CCC1(CCNCC1)C2
HO-
C(C)O
null
null
CC(=O)N1CCC2(CCc3ccc(NS(C)(=O)=O)cc3C2=O)CC1>C(C)O>CS(=O)(=O)Nc1ccc2c(c1)C(=O)C1(CCNCC1)CC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-497ce0dac18148448d14e82b382fc215
c1ccc(CN2CCCC3(Cc4ccccc4O3)C2)cc1>>c1ccc2c(c1)CC1(CCCNC1)O2
C(C1=CC=CC=C1)N1CC2(CCC1)OC1=C(C2)C=CC=C1.ClC(C)OC(=O)Cl>>N1CC2(CCC1)OC1=C(C2)C=CC=C1
c1ccc(C[N:12]2[CH2:11][CH2:10][CH2:9][C:8]3([CH2:7][c:5]4[c:4]([cH:3][cH:2][cH:1][cH:6]4)[O:14]3)[CH2:13]2)cc1>>[cH:1]1[cH:2][cH:3][c:4]2[c:5]([cH:6]1)[CH2:7][C:8]1([CH2:9][CH2:10][CH2:11][NH:12][CH2:13]1)[O:14]2
c1ccc(CN2CCCC3(Cc4ccccc4O3)C2)cc1
c1ccc2c(c1)CC1(CCCNC1)O2
null
null
ClC(C)Cl
Deprotection
Hydrogenolysis of tertiary amines
1026015d984d7b2d2f7382796918788fa1ecd79e4b2ec66ef8b8a45af2877fa7
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
c1ccc2c(c1)CC1(CCCNC1)O2
[#8:1]-[C:2]-[C:3]-[N;H0;D3;+0:4](-C-c1:c:c:c:c:c:1)-[C:5]-[C:6]>>[#8:1]-[C:2]-[C:3]-[NH;D2;+0:4]-[C:5]-[C:6]
94.2
[{"value": 94.2, "product": "N1CC2(CCC1)OC1=C(C2)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 13 g (46 mmole) of 1'-benzyl-2,3-dihydrospiro(benzofuran-2,3'-piperidine) in 100 mL dichloroethane was treated with 7.31 g (5.2 mL, 51 mmoles) of 1-chloroethylchloroformate at room temperature for 1/2 hour. The reaction mixture was concentrated and the residue dissolved in CH3OH and heated to reflux for 1...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.c1ccc2c(c1)CC1(CCC[NH]C1)O2
c1ccc2c(c1)CC1(CCCNC1)O2
c1ccc2c(c1)CC1(CCCNC1)O2
Other
ClC(C)Cl
null
null
c1ccc(CN2CCCC3(Cc4ccccc4O3)C2)cc1>ClC(C)Cl>c1ccc2c(c1)CC1(CCCNC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-898d32e6ca3b42fd8dca89c85c0414f7
CC(=O)N1CCCC2(Cc3cc(NS(C)(=O)=O)ccc3O2)C1>>CS(=O)(=O)Nc1ccc2c(c1)CC1(CCCNC1)O2
C(C)(=O)N1CC2(CCC1)OC1=C(C2)C=C(C=C1)NS(=O)(=O)C.Cl>>Cl.CS(=O)(=O)NC=1C=CC2=C(CC3(CNCCC3)O2)C1
CC(=O)[N:17]1[CH2:16][CH2:15][CH2:14][C:13]2([CH2:12][c:10]3[c:9]([cH:8][cH:7][c:6]([NH:5][S:2]([CH3:1])(=[O:3])=[O:4])[cH:11]3)[O:19]2)[CH2:18]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[CH2:12][C:13]1([CH2:14][CH2:15][CH2:16][NH:17][CH2:18]1)[O:19]2
CC(=O)N1CCCC2(Cc3cc(NS(C)(=O)=O)ccc3O2)C1
CS(=O)(=O)Nc1ccc2c(c1)CC1(CCCNC1)O2
null
null
C(C)O
Reduction
Hydrogenolysis of tertiary amines
1dd4a4692504beab3ace65d954d95be83e12049235aae9a5a01d0ed1c877d2f6
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
c1ccc2c(c1)CC1(CCCNC1)O2
C-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]-[#8:6]>>[#8:6]-[C:5]-[C:4]-[NH;D2;+0:1]-[C:2]-[C:3]
null
[]
null
null
null
null
A solution of 3.6 g (11.09 mmole) of 1'-Acetyl-2,3-dihydro-5-methanesulfonamidospiro(benzofuran-2,3'-piperidine) in 100 mL ethanol was treated with 50 mL 6 N hydrochloric acid and heated to reflux for 18 hours. The reaction was concentrated to dryness and the residue crystallized from ethanol to give 2.77 g of products...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccc2c(c1)CC1(CCC[NH]C1)O2
c1ccc2c(c1)CC1(CCCNC1)O2
c1ccc2c(c1)CC1(CCCNC1)O2
HO-
C(C)O
null
null
CC(=O)N1CCCC2(Cc3cc(NS(C)(=O)=O)ccc3O2)C1>C(C)O>CS(=O)(=O)Nc1ccc2c(c1)CC1(CCCNC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-65ca1e4e59264f35b5d4a1e71549ea75
CS(=O)(=O)Nc1ccc(CCOS(C)(=O)=O)cc1.O=C1CC2(CCCNC2)Oc2ccccc21>>CS(=O)(=O)Nc1ccc(CCN2CCCC3(CC(=O)c4ccccc4O3)C2)cc1
C([O-])(O)=O.[Na+].C(C(=O)O)(=O)O.N1CC2(CCC1)OC1=C(C(C2)=O)C=CC=C1.S(C)(=O)(=O)OCCC1=CC=C(C=C1)NS(=O)(=O)C.C([O-])(O)=O.[Na+]>>C(C(=O)O)(=O)O.CS(=O)(=O)NC1=CC=C(C=C1)CCN1CC2(CCC1)OC1=C(C(C2)=O)C=CC=C1
CS(=O)(=O)O[CH2:11][CH2:10][c:9]1[cH:8][cH:7][c:6]([NH:5][S:2]([CH3:1])(=[O:3])=[O:4])[cH:29][cH:28]1.[NH:12]1[CH2:13][CH2:14][CH2:15][C:16]2([CH2:17][C:18](=[O:19])[c:20]3[cH:21][cH:22][cH:23][cH:24][c:25]3[O:26]2)[CH2:27]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]([CH2:10][CH2:11][N:12]2[CH2:13][CH2:...
CS(=O)(=O)Nc1ccc(CCOS(C)(=O)=O)cc1.O=C1CC2(CCCNC2)Oc2ccccc21
CS(=O)(=O)Nc1ccc(CCN2CCCC3(CC(=O)c4ccccc4O3)C2)cc1
null
null
C(C)O
Heteroatom Alkylation and Arylation
Alkylation of amines
c07f3c636c847819d4f9c223819232dae13e0870974641de199c668de8a7ed5a
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=C1CC2(CCCN(CCc3ccccc3)C2)Oc2ccccc21
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[c:3].[#8:4]-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]>>[#8:4]-[C:5]-[C:6]-[N;H0;D3;+0:7](-[CH2;D2;+0:1]-[C:2]-[c:3])-[C:8]-[C:9]
null
[]
null
null
null
null
A solution of 560 mg (258 mmole) of 3,4-dihydrospiro-[(2H)-1-benzopyran-2,3'-piperidine]4-one in 20 mL ethanol was treated with 880 mg (3 mmoles) of 2-(4-methanesulfonamidophenyl)ethyl mesylate and 0.5 g sodium bicarbonate and heated to reflux for 48 hours. The reaction was cooled to room temperature, poured into satur...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
c1ccc2c(c1)CCC1(CCCNC1)O2
c1ccc2c(c1)CCC1(CCC[NH]C1)O2
c1ccccc1.c1ccc2c(c1)CCC1(CCC[NH]C1)O2
MsOH.HO-
C(C)O
null
null
CS(=O)(=O)Nc1ccc(CCOS(C)(=O)=O)cc1.O=C1CC2(CCCNC2)Oc2ccccc21>C(C)O>CS(=O)(=O)Nc1ccc(CCN2CCCC3(CC(=O)c4ccccc4O3)C2)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-6aeb04d026c546f9b1095e74fc25312b
CC(Cl)OC(=O)Cl.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCCN(Cc3ccccc3)C1)O2>>CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCCNC1)O2.Cl
C([O-])(O)=O.[Na+].CS(=O)(=O)NC=1C=CC2=C(C(CC3(CN(CCC3)CC3=CC=CC=C3)O2)=O)C1.C(C)(C)N(CC)C(C)C.ClC(=O)OC(C)Cl>>Cl.CS(=O)(=O)NC=1C=CC2=C(C(CC3(CNCCC3)O2)=O)C1
CC(Cl)OC(=O)[Cl:22].c1ccc(C[N:19]2[CH2:18][CH2:17][CH2:16][C:15]3([CH2:14][C:12](=[O:13])[c:10]4[c:9]([cH:8][cH:7][c:6]([NH:5][S:2]([CH3:1])(=[O:3])=[O:4])[cH:11]4)[O:21]3)[CH2:20]2)cc1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[C:12](=[O:13])[CH2:14][C:15]1([CH2:16][CH2:17][CH2:18][NH:...
CC(Cl)OC(=O)Cl.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCCN(Cc3ccccc3)C1)O2
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCCNC1)O2.Cl
null
null
ClC(C)Cl
Miscellaneous
OtherReaction
275fd43c0f08bde74a8898d2475fc1fe25be078812dabd4b8248cda02e1ce012
8680972761abf0bd12e62e23250487041204d99e9f76a29275e470fb95a71c86
O=C1CC2(CCCNC2)Oc2ccccc21
C-C(-Cl)-O-C(=O)-[Cl;H0;D1;+0:1].[#8:2]-[C:3]-[C:4]-[N;H0;D3;+0:5](-C-c1:c:c:c:c:c:1)-[C:6]-[C:7]>>[#8:2]-[C:3]-[C:4]-[NH;D2;+0:5]-[C:6]-[C:7].[ClH;D0;+0:1]
67.7
[{"value": 67.7, "product": "Cl.CS(=O)(=O)NC=1C=CC2=C(C(CC3(CNCCC3)O2)=O)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution of 7 g (17.47 mmols) of 6-methanesulfonamido-1'-benzyl-3,4-dihydrospiro-[(2H)-1-benzopyran-2,3'-piperidine]-4-one in 250 mL dichloroethane was treated with 5.6 g (43.7 mmole) of diisopropylethylamine, and 6.24 g (43.7 mmoles) of 1-chloroethyl chloroformate. The reaction was stirred at room temperature for 24...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary halide.Ether.Tertiary amine
Secondary amine
c1ccccc1.c1ccc2c(c1)CCC1(CCC[NH]C1)O2
c1ccc2c(c1)CCC1(CCCNC1)O2
c1ccc2c(c1)CCC1(CCCNC1)O2
HCl
ClC(C)Cl
null
24
CC(Cl)OC(=O)Cl.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCCN(Cc3ccccc3)C1)O2>ClC(C)Cl>CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCCNC1)O2.Cl
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-929bcdee11ce49d59e2a83b23d640eb8
CC(Cl)OC(=O)Cl.CN1CCC2(CC1)Cc1ccc(NS(C)(=O)=O)cc1CO2>>CS(=O)(=O)Nc1ccc2c(c1)COC1(CCNCC1)C2.Cl
CN1CCC2(CC1)OCC1=C(C2)C=CC(=C1)NS(=O)(=O)C.CN(C1=CC=CC2=CC=CC(=C12)N(C)C)C.ClC(=O)OC(C)Cl>>Cl.CS(=O)(=O)NC1=CC2=C(CC3(CCNCC3)OC2)C=C1
CC(Cl)OC(=O)[Cl:21].C[N:17]1[CH2:16][CH2:15][C:14]2([O:13][CH2:12][c:10]3[c:9]([cH:8][cH:7][c:6]([NH:5][S:2]([CH3:1])(=[O:3])=[O:4])[cH:11]3)[CH2:20]2)[CH2:19][CH2:18]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[CH2:12][O:13][C:14]1([CH2:15][CH2:16][NH:17][CH2:18][CH2:19]1)[CH2:20]2.[Cl...
CC(Cl)OC(=O)Cl.CN1CCC2(CC1)Cc1ccc(NS(C)(=O)=O)cc1CO2
CS(=O)(=O)Nc1ccc2c(c1)COC1(CCNCC1)C2.Cl
null
null
ClC(C)Cl
Miscellaneous
OtherReaction
77ac135b0fa246a6fefda7e08ae112cceb419f1d60863dd6eb2ea9e92853875f
8680972761abf0bd12e62e23250487041204d99e9f76a29275e470fb95a71c86
c1ccc2c(c1)COC1(CCNCC1)C2
C-C(-Cl)-O-C(=O)-[Cl;H0;D1;+0:1].C-[N;H0;D3;+0:2](-[C:3]-[C:4])-[C:5]-[C:6]>>[C:4]-[C:3]-[NH;D2;+0:2]-[C:5]-[C:6].[ClH;D0;+0:1]
null
[]
null
null
null
null
To a solution of 1,4-dihydro-1'-methyl-7-methanesulfonamido-spiro[(3H)-2-benzopyran-3,4'-piperidine](0.575 g) and N,N,N',N'-tetramethyl-1,8-napthalenediamine (proton sponge) (0.6 g) in dichloroethane under nitrogen at 0° C. was added 1-chloroethyl chloroformate (0.613 ml). The mixture was stirred at reflux for 2 hours,...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary halide.Ether.Tertiary amine
Secondary amine
c1ccc2c(c1)COC1(CC[NH]CC1)C2
c1ccc2c(c1)COC1(CCNCC1)C2
c1ccc2c(c1)COC1(CCNCC1)C2
HCl
ClC(C)Cl
null
null
CC(Cl)OC(=O)Cl.CN1CCC2(CC1)Cc1ccc(NS(C)(=O)=O)cc1CO2>ClC(C)Cl>CS(=O)(=O)Nc1ccc2c(c1)COC1(CCNCC1)C2.Cl
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-11292f8d3ee3493ab3e125d923f45655
CC(=O)c1ccccc1O.O=C1CCN(C(=O)c2ccccc2)CC1>>O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Oc2ccccc21
C(C)(=O)C1=C(C=CC=C1)O.C(C1=CC=CC=C1)(=O)N1CCC(CC1)=O.N1CCCC1>>C(C1=CC=CC=C1)(=O)N1CCC2(CC1)OC1=C(C(C2)=O)C=CC=C1
[O:1]=[C:2]([CH3:3])[c:24]1[c:19]([OH:18])[cH:20][cH:21][cH:22][cH:23]1.O=[C:4]1[CH2:5][CH2:6][N:7]([C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)[CH2:16][CH2:17]1>>[O:1]=[C:2]1[CH2:3][C:4]2([CH2:5][CH2:6][N:7]([C:8](=[O:9])[c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[CH2:16][CH2:17]2)[O:18][c:19]2[cH:20][cH...
CC(=O)c1ccccc1O.O=C1CCN(C(=O)c2ccccc2)CC1
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Oc2ccccc21
null
null
CO
Heteroatom Alkylation and Arylation
spiro-chromanone
516e17e36e6da47114ec867780566e28862277ef4db6e563ed68fe6015ca5775
2b19ddad93f276f7cba72518a5f5b44fb4fd6e49b358f1173e7b2c08a31b3f60
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Oc2ccccc21
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1.[CH3;D1;+0:7]-[C:8](=[O;D1;H0:9])-[c:10]:[c:11](-[OH;D1;+0:12]):[c:13]>>[O;D1;H0:9]=[C:8]1-[CH2;D2;+0:7]-[C;H0;D4;+0:1]2(-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-2)-[O;H0;D2;+0:12]-[c:11](:[c:13]):[c:10]-1
68,961.6
[{"value": 68961.6, "product": "C(C1=CC=CC=C1)(=O)N1CCC2(CC1)OC1=C(C(C2)=O)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 2-acetylphenol (5 g, 0.037 mmol), 1-benzoyl-4-piperidone (7.5 g, 0.037 mmol), pyrrolidine (2.6 g, 0.037 mol) and CH3OH (50 ml) was heated at reflux for 8 hours. After cooling to room temperature overnight, the solid was filtered to yield 8.2 g of 1'-benzoyl-3,4-dihydro-spiro[(2H)-1-benzopyran-2,4'-piperid...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone.Aromatic alcohol
Ketone.Ether
C1CC[NH]CC1
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccccc1.c1ccc2c(c1)CCC1(CC[NH]CC1)O2
HO-
CO
null
null
CC(=O)c1ccccc1O.O=C1CCN(C(=O)c2ccccc2)CC1>CO>O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Oc2ccccc21
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-f5952f2d3c1a47b8a5eff37ecec2b712
CN1CCC2(CC1)CC(=O)c1ccccc1O2.O=[N+]([O-])O>>CN1CCC2(CC1)CC(=O)c1cc([N+](=O)[O-])ccc1O2
C(C)(=O)OCC.C([O-])(O)=O.[Na+].CN1CCC2(CC1)OC1=C(C(C2)=O)C=CC=C1.[N+](=O)(O)[O-].[N+](=O)(O)[O-]>>CN1CCC2(CC1)OC1=C(C(C2)=O)C=C(C=C1)[N+](=O)[O-]
[CH3:1][N:2]1[CH2:3][CH2:4][C:5]2([CH2:6][CH2:7]1)[CH2:8][C:9](=[O:10])[c:11]1[cH:12][cH:13][cH:17][cH:18][c:19]1[O:20]2.O[N+:14](=[O:15])[O-:16]>>[CH3:1][N:2]1[CH2:3][CH2:4][C:5]2([CH2:6][CH2:7]1)[CH2:8][C:9](=[O:10])[c:11]1[cH:12][c:13]([N+:14](=[O:15])[O-:16])[cH:17][cH:18][c:19]1[O:20]2
CN1CCC2(CC1)CC(=O)c1ccccc1O2.O=[N+]([O-])O
CN1CCC2(CC1)CC(=O)c1cc([N+](=O)[O-])ccc1O2
null
null
S(O)(O)(=O)=O
Functional Group Addition
Aromatic nitration with HNO3
3e8bba8cfd479ea26838cd4df10d0b1719e48d1515854da8f965d36d40f55885
ddce49825c02b8965f10c8d99e3c841d26e1f136da6037b417c09313e6d73097
O=C1CC2(CCNCC2)Oc2ccccc21
O-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3].[O;D1;H0:4]=[C:5]-[c:6]:[c:7]:[cH;D2;+0:8]:[c:9]:[c:10]>>[O;-;D1;H0:2]-[N+;H0;D3:1](=[O;D1;H0:3])-[c;H0;D3;+0:8](:[c:7]:[c:6]-[C:5]=[O;D1;H0:4]):[c:9]:[c:10]
77
[{"value": 77.0, "product": "CN1CCC2(CC1)OC1=C(C(C2)=O)C=C(C=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 76.7, "product": "CN1CCC2(CC1)OC1=C(C(C2)=O)C=C(C=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
Sulfuric acid (55 ml) was cooled to 0° C. and was stirred as 3,4-dihydro-1'-methyl-spiro[2H-1-benzopyran-2,4'-piperidin]-4-one (11.56 g, 0.05 mol) was added over 20 minutes. Some gum separated. A solution of 90% nitric acid (2.5 ml, 0.0525 mol) in sulfuric acid (5 ml) was added over 20 minutes. The mixture was stirred ...
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
HO-
S(O)(O)(=O)=O
0
2
CN1CCC2(CC1)CC(=O)c1ccccc1O2.O=[N+]([O-])O>S(O)(O)(=O)=O>CN1CCC2(CC1)CC(=O)c1cc([N+](=O)[O-])ccc1O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-b71bc264b15d49928dd81de121d205e8
CN1CCC2(CC1)CC(=O)c1cc([N+](=O)[O-])ccc1O2>>CN1CCC2(CC1)CC(=O)c1cc(N)ccc1O2
CN1CCC2(CC1)OC1=C(C(C2)=O)C=C(C=C1)[N+](=O)[O-]>>NC=1C=CC2=C(C(CC3(CCN(CC3)C)O2)=O)C1
O=[N+:14]([O-])[c:13]1[cH:12][c:11]2[c:17]([cH:16][cH:15]1)[O:18][C:5]1([CH2:4][CH2:3][N:2]([CH3:1])[CH2:7][CH2:6]1)[CH2:8][C:9]2=[O:10]>>[CH3:1][N:2]1[CH2:3][CH2:4][C:5]2([CH2:6][CH2:7]1)[CH2:8][C:9](=[O:10])[c:11]1[cH:12][c:13]([NH2:14])[cH:15][cH:16][c:17]1[O:18]2
CN1CCC2(CC1)CC(=O)c1cc([N+](=O)[O-])ccc1O2
CN1CCC2(CC1)CC(=O)c1cc(N)ccc1O2
null
[Ni]
C(C)(=O)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C1CC2(CCNCC2)Oc2ccccc21
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
75.1
[{"value": 75.0, "product": "NC=1C=CC2=C(C(CC3(CCN(CC3)C)O2)=O)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.1, "product": "NC=1C=CC2=C(C(CC3(CCN(CC3)C)O2)=O)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The 3,4-dihydro-1'-methyl-6-nitro-spiro[2H-1-benzopyran-2,4'-piperdin]-4-one (11.2 g, 0.04 mol) was dissolved in acetic acid (200 ml) and was hydrogenated using two "lab spoon" spatulas of Raney nickel catalyst in a Parr shaker. The theoretical amount of hydrogen was absorbed in 4 hours. The reaction mixture was filter...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
Other
[Ni].C(C)(=O)O
null
null
CN1CCC2(CC1)CC(=O)c1cc([N+](=O)[O-])ccc1O2>[Ni].C(C)(=O)O>CN1CCC2(CC1)CC(=O)c1cc(N)ccc1O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-6c24fe13f1134a09b0896f1b0f8ba6a0
CN1CCC2(CC1)CC(=O)c1cc(N)ccc1O2.CS(=O)(=O)Cl>>CN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2
NC=1C=CC2=C(C(CC3(CCN(CC3)C)O2)=O)C1.N1=CC=CC=C1.CS(=O)(=O)Cl>>CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)C)O2)=O)C1
[CH3:1][N:2]1[CH2:3][CH2:4][C:5]2([CH2:6][CH2:7]1)[CH2:8][C:9](=[O:10])[c:11]1[cH:12][c:13]([NH2:14])[cH:19][cH:20][c:21]1[O:22]2.Cl[S:15]([CH3:16])(=[O:17])=[O:18]>>[CH3:1][N:2]1[CH2:3][CH2:4][C:5]2([CH2:6][CH2:7]1)[CH2:8][C:9](=[O:10])[c:11]1[cH:12][c:13]([NH:14][S:15]([CH3:16])(=[O:17])=[O:18])[cH:19][cH:20][c:21]1[...
CN1CCC2(CC1)CC(=O)c1cc(N)ccc1O2.CS(=O)(=O)Cl
CN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2
null
null
C(Cl)Cl
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
O=C1CC2(CCNCC2)Oc2ccccc21
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[C;D1;H3:2]-[S;H0;D4;+0:1](=[O;D1;H0:3])(=[O;D1;H0:4])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]
419
[{"value": 50.0, "product": "CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)C)O2)=O)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 419.0, "product": "CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)C)O2)=O)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
3,4-Dihydro-6-amino-1'-methyl-spiro[2H-1-benzopyran-2,4'-piperidin]-4-one (5.6 g, 0.0027 mol) was stirred in methylene chloride (50 ml) and pyridine (16 ml) at room temperature under a nitrogen atmosphere as methanesulfonyl chloride (2.7 ml, 0.035 mol) was added dropwise over several minutes. Some gum separated so addi...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
HCl
C(Cl)Cl
null
16
CN1CCC2(CC1)CC(=O)c1cc(N)ccc1O2.CS(=O)(=O)Cl>C(Cl)Cl>CN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-442301e70e88430aba7d194beb8dd46d
COC(=O)C=P(c1ccccc1)(c1ccccc1)c1ccccc1.O=C1CCN(C(=O)c2ccccc2)CC1>>O=P(c1ccccc1)(c1ccccc1)c1ccccc1
C(C1=CC=CC=C1)(=O)N1CCC(CC1)=O.COC(=O)C=P(C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3>>C1(=CC=CC=C1)P(C1=CC=CC=C1)(C1=CC=CC=C1)=O
COC(=O)C=[P:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1)([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.O=C1CCN(C(c2ccccc2)=[O:1])CC1>>[O:1]=[P:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1)([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
COC(=O)C=P(c1ccccc1)(c1ccccc1)c1ccccc1.O=C1CCN(C(=O)c2ccccc2)CC1
O=P(c1ccccc1)(c1ccccc1)c1ccccc1
null
null
C1(=CC=CC=C1)C
Miscellaneous
OtherReaction
b2358a42b6497fe7f75dece333a35a7d4e164eab9b78bc1466d704ff9aa32ca2
ed6b3c2c64f30232911a85c601dabf2ab8cc0203e565c0f182ba92f19c27f5b0
O=P(c1ccccc1)(c1ccccc1)c1ccccc1
C-O-C(=O)-C=[P;H0;D4;+0:1](-[c:2](:[c:3]):[c:4])(-[c:5](:[c:6]):[c:7])-[c:8](:[c:9]):[c:10].O=C1-C-C-N(-C(=[O;H0;D1;+0:11])-c2:c:c:c:c:c:2)-C-C-1>>[O;H0;D1;+0:11]=[P;H0;D4;+0:1](-[c:2](:[c:3]):[c:4])(-[c:5](:[c:6]):[c:7])-[c:8](:[c:9]):[c:10]
100
[{"value": 100.0, "product": "C1(=CC=CC=C1)P(C1=CC=CC=C1)(C1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.9, "product": "C1(=CC=CC=C1)P(C1=CC=CC=C1)(C1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Under N2, a mixture of 1-benzoyl-4-piperidone (10.2 g, 0.05 mol), methyl (triphenylphosphoranylidene) acetate (25 g. 0.074 mol) in toluene (100 ml) was heated at reflux for 7 hours. After stirring at room temperature overnight, the solid was filtered off to yield 13.9 g (100%) of triphenylphosphine oxide. The mother li...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Tertiary amide
null
C1CCNCC1.c1ccccc1
null
c1ccccc1.c1ccccc1.c1ccccc1
HO-
C1(=CC=CC=C1)C
null
8
COC(=O)C=P(c1ccccc1)(c1ccccc1)c1ccccc1.O=C1CCN(C(=O)c2ccccc2)CC1>C1(=CC=CC=C1)C>O=P(c1ccccc1)(c1ccccc1)c1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-16fafd1fac294152bba99cdec776ba37
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2ccccc21>>O=C1CC2(CCNCC2)Sc2ccccc21
C(C1=CC=CC=C1)(=O)N1CCC2(CC1)SC1=C(C(C2)=O)C=CC=C1.Cl>>N1CCC2(CC1)SC1=C(C(C2)=O)C=CC=C1.Cl
O=C(c1ccccc1)[N:8]1[CH2:7][CH2:6][C:5]2([CH2:4][C:3](=[O:2])[c:17]3[c:12]([cH:13][cH:14][cH:15][cH:16]3)[S:11]2)[CH2:10][CH2:9]1>>[O:2]=[C:3]1[CH2:4][C:5]2([CH2:6][CH2:7][NH:8][CH2:9][CH2:10]2)[S:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]21
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2ccccc21
O=C1CC2(CCNCC2)Sc2ccccc21
null
null
C(C)O
Reduction
Hydrogenolysis of tertiary amines
d1ebdb22415b26584cd851599e266cb438c3b635953aed3fef73bc2af0a7785e
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
O=C1CC2(CCNCC2)Sc2ccccc21
O=C(-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5])-c1:c:c:c:c:c:1>>[C:5]-[C:4]-[NH;D2;+0:1]-[C:2]-[C:3]
92
[{"value": 92.0, "product": "N1CCC2(CC1)SC1=C(C(C2)=O)C=CC=C1.Cl", "details": "PERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of product from Step C (3.2 g, 0.0095 mol) in ethanol (50 ml) and 6 N HCl (50 ml) was heated at reflux. After 18 hours, the reaction was concentrated to dryness and the residue crystallized from ethanol to yield 2.9 g (92%) of product. Conditions: See reaction.notes.procedure_details. Workup: at reflux; the ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccccc1.c1ccc2c(c1)CCC1(CC[NH]CC1)S2
c1ccc2c(c1)CCC1(CCNCC1)S2
c1ccc2c(c1)CCC1(CCNCC1)S2
HO-
C(C)O
null
18
O=C1CC2(CCN(C(=O)c3ccccc3)CC2)Sc2ccccc21>C(C)O>O=C1CC2(CCNCC2)Sc2ccccc21
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a4e3b11bcb904ad0ac7556437318ff19
O=C1CCN(C(=O)c2ccccc2)CC1.Sc1ccccc1S>>O=C(c1ccccc1)N1CCC2(CC1)Sc1ccccc1S2
[O-]S(=O)(=O)[O-].[Na+].[Na+].SC1=C(C=CC=C1)S.C(C1=CC=CC=C1)(=O)N1CCC(CC1)=O.Cl>>C(C1=CC=CC=C1)(=O)N1CCC2(CC1)SC1=C(S2)C=CC=C1
O=[C:12]1[CH2:11][CH2:10][N:9]([C:2](=[O:1])[c:3]2[cH:4][cH:5][cH:6][cH:7][cH:8]2)[CH2:14][CH2:13]1.[SH:15][c:16]1[cH:17][cH:18][cH:19][cH:20][c:21]1[SH:22]>>[O:1]=[C:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1)[N:9]1[CH2:10][CH2:11][C:12]2([CH2:13][CH2:14]1)[S:15][c:16]1[cH:17][cH:18][cH:19][cH:20][c:21]1[S:22]2
O=C1CCN(C(=O)c2ccccc2)CC1.Sc1ccccc1S
O=C(c1ccccc1)N1CCC2(CC1)Sc1ccccc1S2
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
OtherReaction
0d3b18413d76e6e4f42668a3203734c6ab13511bbbeed5b7442e4129cf2c9c7f
1d9d6ee9d77442dc1bde18cc35949be811ff28784f0810fab70dac59f3531b1b
O=C(c1ccccc1)N1CCC2(CC1)Sc1ccccc1S2
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1.[SH;D1;+0:7]-[c:8](:[c:9]):[c:10](-[SH;D1;+0:11]):[c:12]>>[c:9]:[c:8]1:[c:10](:[c:12])-[S;H0;D2;+0:11]-[C;H0;D4;+0:1]2(-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-2)-[S;H0;D2;+0:7]-1
null
[]
null
null
15
HOUR
500 mgs (3.52 mmol) of 1,2-dimercaptobenzene and 610 mgs (3.00 mmol) of N-benzoyl-4-piperidone were stirred in CH2Cl2 while anhydrous HCl gas was introduced Na2SO4 (2 grams) was added and the mixture stirred 15 hours. The mixture was diluted with CH2Cl2 filtered and washed with H2O, and 10% NaOH. The organics were drie...
10.6084/m9.figshare.5104873.v1
null
Ketone.Aromatic thiol.Aromatic thiol
Monosulfide.Monosulfide
C1CC[NH]CC1
c1ccc2c(c1)SC1(CC[NH]CC1)S2
c1ccccc1.c1ccc2c(c1)SC1(CC[NH]CC1)S2
HO-
C(Cl)Cl
null
15
O=C1CCN(C(=O)c2ccccc2)CC1.Sc1ccccc1S>C(Cl)Cl>O=C(c1ccccc1)N1CCC2(CC1)Sc1ccccc1S2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-25efeb1467b543d6aa08ef96cec87305
O=C(c1ccccc1)N1CCC2(CC1)Sc1ccc([N+](=O)[O-])cc1S2>>O=[N+]([O-])c1ccc2c(c1)SC1(CCNCC1)S2
[N+](=O)([O-])C1=CC2=C(SC3(CCN(CC3)C(C3=CC=CC=C3)=O)S2)C=C1.[OH-].[Na+]>>[N+](=O)([O-])C1=CC2=C(SC3(CCNCC3)S2)C=C1
O=C(c1ccccc1)[N:14]1[CH2:13][CH2:12][C:11]2([S:10][c:8]3[c:7]([cH:6][cH:5][c:4]([N+:2](=[O:1])[O-:3])[cH:9]3)[S:17]2)[CH2:16][CH2:15]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]2[c:8]([cH:9]1)[S:10][C:11]1([CH2:12][CH2:13][NH:14][CH2:15][CH2:16]1)[S:17]2
O=C(c1ccccc1)N1CCC2(CC1)Sc1ccc([N+](=O)[O-])cc1S2
O=[N+]([O-])c1ccc2c(c1)SC1(CCNCC1)S2
null
null
O.C(C)O
Reduction
Hydrogenolysis of tertiary amines
7a4d431ad2c3398f8b9b7205e7987bcd97785cc9e17c383f46bf55db87ca5662
62cf08a8ae6315067a063b5b3495125ccbdaff6b2340ce1d3e1c7b6cde962ae4
c1ccc2c(c1)SC1(CCNCC1)S2
O=C(-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5])-c1:c:c:c:c:c:1>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
70
CELSIUS
null
null
1.20 grams of the nitro dithioacetal from Step B in 46 mL of ethanol was treated with 18 mL of 40% aqueous NaOH and heated to 70° C. for 8 hours. The solution was diluted with water and extracted with CH2Cl2. The organics were combined, washed with water, saturated aqueous sodium carbonate, brine, dried (Na2SO4) and co...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Secondary amine
c1ccccc1.c1ccc2c(c1)SC1(CC[NH]CC1)S2
c1ccc2c(c1)SC1(CCNCC1)S2
c1ccc2c(c1)SC1(CCNCC1)S2
HO-
O.C(C)O
70
null
O=C(c1ccccc1)N1CCC2(CC1)Sc1ccc([N+](=O)[O-])cc1S2>O.C(C)O>O=[N+]([O-])c1ccc2c(c1)SC1(CCNCC1)S2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-31cfffa70224479c92ad749173c818db
O=[N+]([O-])c1ccc(CCBr)cc1.c1ccc2c(c1)CSC1(CCNCC1)S2>>O=[N+]([O-])c1ccc(CC[SH]2c3ccccc3CSC23CCNCC3)cc1
N1CCC2(CC1)SC1=C(CS2)C=CC=C1.C([O-])(O)=O.[Na+].[N+](=O)([O-])C1=CC=C(C=C1)CCBr>>[N+](=O)([O-])C1=CC=C(C=C1)CCS1C2=C(CSC13CCNCC3)C=CC=C2
Br[CH2:9][CH2:8][c:7]1[cH:6][cH:5][c:4]([N+:2](=[O:1])[O-:3])[cH:26][cH:25]1.[S:10]1[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[CH2:17][S:18][C:19]12[CH2:20][CH2:21][NH:22][CH2:23][CH2:24]2>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([CH2:8][CH2:9][SH:10]2[c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[CH2:17][S:18][C:19]23...
O=[N+]([O-])c1ccc(CCBr)cc1.c1ccc2c(c1)CSC1(CCNCC1)S2
O=[N+]([O-])c1ccc(CC[SH]2c3ccccc3CSC23CCNCC3)cc1
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
a51cb16fe989549697d0fa051a0b9360266beb43e42e8c0dd6050e627f0ceccf
1e6339d75322cc45c770cf1fc8fe9638f88f9eff36385ca6e4f82c8cab3a96f8
c1ccc(CC[SH]2c3ccccc3CSC23CCNCC3)cc1
Br-[CH2;D2;+0:1]-[C:2]-[c:3].[C:4]-[C:5]1(-[C:6])-[#16:7]-[C:8]-[c:9]:[c:10](:[c:11])-[S;H0;D2;+0:12]-1>>[C:4]-[C:5]1(-[C:6])-[#16:7]-[C:8]-[c:9]:[c:10](:[c:11])-[SH;D3;+0:12]-1-[CH2;D2;+0:1]-[C:2]-[c:3]
null
[]
null
null
null
null
To 111 mgs (0.47 mmol) of dithioketal from Step A in 1 mL of methanol was added 157 mgs of sodium bicarbonate and 118 mg (0.54 mmol) of 2-(4-nitrophenyl)ethyl bromide. The reaction was refluxed for 6 hrs and then concentrated at reduced pressure. The residue was chromotographed (silica gel, 2.5% CH3OH/CH2Cl2) to give a...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Monosulfide
null
c1ccc2c(c1)CSC1(CCNCC1)S2
c1ccc2c(c1)CSC1(CCNCC1)[SH]2
c1ccccc1.c1ccc2c(c1)CSC1(CCNCC1)[SH]2
Br-
CO
null
null
O=[N+]([O-])c1ccc(CCBr)cc1.c1ccc2c(c1)CSC1(CCNCC1)S2>CO>O=[N+]([O-])c1ccc(CC[SH]2c3ccccc3CSC23CCNCC3)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-21f4820d09ec43eea37f1383b4e918e9
O=C1CCNC(CCc2ccccn2)C1.O=[N+]([O-])c1ccc(S)c(CO)c1>>O=[N+]([O-])c1ccc2c(c1)COC1(CCN(CCc3ccccn3)CC1)S2
SC1=C(CO)C=C(C=C1)[N+](=O)[O-].N1=C(C=CC=C1)CCC1NCCC(C1)=O>>[N+](=O)([O-])C=1C=CC2=C(COC3(CCN(CC3)CCC3=NC=CC=C3)S2)C1
O=[C:12]1[CH2:13][CH2:14][NH:15][CH:24]([CH2:16][CH2:17][c:18]2[cH:19][cH:20][cH:21][cH:22][n:23]2)[CH2:25]1.[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([SH:26])[c:8]([CH2:10][OH:11])[cH:9]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]2[c:8]([cH:9]1)[CH2:10][O:11][C:12]1([CH2:13][CH2:14][N:15]([CH2:16][CH2:17][c:18]3[c...
O=C1CCNC(CCc2ccccn2)C1.O=[N+]([O-])c1ccc(S)c(CO)c1
O=[N+]([O-])c1ccc2c(c1)COC1(CCN(CCc3ccccn3)CC1)S2
null
null
C(Cl)(Cl)Cl
Functional Group Addition
OtherReaction
da0f6fb37cfbac9efa5ed795a217be23806f6e418aa769761a4132f58e2bd279
4118bbf535066e47681c317ea46590ac414fddca620ebd1df5edc56214153d73
c1ccc(CCN2CCC3(CC2)OCc2ccccc2S3)nc1
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[NH;D2;+0:4]-[CH;D3;+0:5](-[CH2;D2;+0:6]-[C:7]-[c:8]:[#7;a:9])-[C:10]-1.[OH;D1;+0:11]-[C:12]-[c:13]:[c:14](-[SH;D1;+0:15]):[c:16]>>[#7;a:9]:[c:8]-[C:7]-[CH2;D2;+0:6]-[N;H0;D3;+0:4]1-[C:3]-[C:2]-[C;H0;D4;+0:1]2(-[C:10]-[CH2;D2;+0:5]-1)-[O;H0;D2;+0:11]-[C:12]-[c:13]:[c:14](:[c:16])-[S;H0;D2;...
null
[]
25
CELSIUS
2
DAY
2-Mercapto-5-nitrobenzyl alcohol (150 mg, 0.81 mmol) and 208 mg (0.80 mm) of N-[2-(2'-pyridyl ethyl]-4-piperidone was dissolved in 5 mL of CHCl3. HCl Gas was bubbled in to saturate the solution, the mixture stirred at 25° C. for 2 days, then diluted with water and the pH adjusted to 10.0 with 40% aqueous NaOH. Extracti...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary alcohol.Secondary amine.Aromatic thiol
Ether.Tertiary amine.Monosulfide
C1CCNCC1
c1ccc2c(c1)COC1(CC[NH]CC1)S2
c1ccc2c(c1)COC1(CC[NH]CC1)S2.c1ccncc1
HO-
C(Cl)(Cl)Cl
25
48
O=C1CCNC(CCc2ccccn2)C1.O=[N+]([O-])c1ccc(S)c(CO)c1>C(Cl)(Cl)Cl>O=[N+]([O-])c1ccc2c(c1)COC1(CCN(CCc3ccccn3)CC1)S2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-09b8475db80c4c40aa60750fe9e33c66
CS(=O)(=O)Cl.OCCc1ccc2nonc2c1>>CS(=O)(=O)OCCc1ccc2nonc2c1
OCCC=1C=CC=2C(=NON2)C1.C(C)N(CC)CC.CS(=O)(=O)Cl>>CS(=O)(=O)OCCC=1C=CC=2C(=NON2)C1
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][CH2:7][c:8]1[cH:9][cH:10][c:11]2[n:12][o:13][n:14][c:15]2[cH:16]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][CH2:7][c:8]1[cH:9][cH:10][c:11]2[n:12][o:13][n:14][c:15]2[cH:16]1
CS(=O)(=O)Cl.OCCc1ccc2nonc2c1
CS(=O)(=O)OCCc1ccc2nonc2c1
null
null
ClCCl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1ccc2nonc2c1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6]-[OH;D1;+0:7]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
96.3
[{"value": 96.0, "product": "CS(=O)(=O)OCCC=1C=CC=2C(=NON2)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.3, "product": "CS(=O)(=O)OCCC=1C=CC=2C(=NON2)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-30
CELSIUS
15
MINUTE
5-(2-Hydroxyethyl)benzofurazan (1.48 g, 9 mmol) was dissolved in dichloromethane (45 ml) and triethylamine (1.88 ml, 1.37 g, 13.5 mmol) was added. The mixture was cooled to -30° C. and methanesulfonyl chloride (0.84 ml, 1.24 g, 10.8 mmol) was added dropwise over 5 min. The mixture was stirred at -30° C. for 15 min. and...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1ccc2nonc2c1
HCl
ClCCl
-30
0.25
CS(=O)(=O)Cl.OCCc1ccc2nonc2c1>ClCCl>CS(=O)(=O)OCCc1ccc2nonc2c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-3a716ce8682049ba850c6a9e0138388f
BrCCBr.Oc1ccc2nonc2c1>>BrCCOc1ccc2nonc2c1
[OH-].[Na+].OC=1C=CC=2C(=NON2)C1.BrCCBr>>BrCCOC=1C=CC=2C(=NON2)C1
Br[CH2:3][CH2:2][Br:1].[OH:4][c:5]1[cH:6][cH:7][c:8]2[n:9][o:10][n:11][c:12]2[cH:13]1>>[Br:1][CH2:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8]2[n:9][o:10][n:11][c:12]2[cH:13]1
BrCCBr.Oc1ccc2nonc2c1
BrCCOc1ccc2nonc2c1
null
null
C(C)O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccc2nonc2c1
Br-[CH2;D2;+0:1]-[C:2]-[Br;D1;H0:3].[#7;a:4]:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]>>[#7;a:4]:[c:5]:[c:6]:[c:7](-[O;H0;D2;+0:8]-[CH2;D2;+0:1]-[C:2]-[Br;D1;H0:3]):[c:9]
41
[{"value": 41.0, "product": "BrCCOC=1C=CC=2C(=NON2)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 40.7, "product": "BrCCOC=1C=CC=2C(=NON2)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Sodium hydroxide (40 mg, 1 mmol) was added to a solution of 5-hydroxybenzofurazan (136 mg, 1 mmol) in ethanol (2 ml) and the mixture was stirred at room temperature for 30 min. 1,2-dibromoethane (0.26 ml, 0.56 g, 3 mmol) was added and the mixture was heated under reflux for 20 hr., cooled and the solvent was evaporated...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccc2nonc2c1
HBr
C(C)O
null
0.5
BrCCBr.Oc1ccc2nonc2c1>C(C)O>BrCCOc1ccc2nonc2c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a044b14d95534fccb6fff56c706226ca
BrC(Br)(Br)Br.OCCc1ccc2nonc2c1>>BrCCc1ccc2nonc2c1
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.OCCC=1C=CC=2C(=NON2)C1.C(Br)(Br)(Br)Br>>BrCCC=1C=CC=2C(=NON2)C1
BrC(Br)(Br)[Br:1].O[CH2:2][CH2:3][c:4]1[cH:5][cH:6][c:7]2[n:8][o:9][n:10][c:11]2[cH:12]1>>[Br:1][CH2:2][CH2:3][c:4]1[cH:5][cH:6][c:7]2[n:8][o:9][n:10][c:11]2[cH:12]1
BrC(Br)(Br)Br.OCCc1ccc2nonc2c1
BrCCc1ccc2nonc2c1
null
null
C(Cl)Cl
Functional Group Interconversion
Appel reaction
752e1807cd47d8316010cc3f92eab16c5a89ffb844d9514fcae469ba993c78dd
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
c1ccc2nonc2c1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3]-[c:4]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3]-[c:4]
86,639,240
[{"value": 86.0, "product": "BrCCC=1C=CC=2C(=NON2)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86639240.0, "product": "BrCCC=1C=CC=2C(=NON2)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
A solution of 5-(2-hydroxyethyl)benzofurazan (1.0 g, 6.1 nmol) and carbon tetrabromide (2.6 g, 7.9 nmol) in methylene chloride (10 ml) was cooled to 0° C. A solution of triphenyl phosphine (1.9 g, 7.3 nmol) in methylene chloride (10 ml) was added dropwise and the reaction was stirred for 5 min. Solvent evaporation and ...
10.6084/m9.figshare.5104873.v1
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Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
null
null
c1ccc2nonc2c1
HBr
C(Cl)Cl
null
0.083333
BrC(Br)(Br)Br.OCCc1ccc2nonc2c1>C(Cl)Cl>BrCCc1ccc2nonc2c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-6d12d6442a96446d8a9c31f411e01809
BrCCc1ccc2nonc2c1.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2>>CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc4nonc4c3)CC1)O2
BrCCC=1C=CC=2C(=NON2)C1.Cl.CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCNCC3)O2)=O)C1.C([O-])(O)=O.[Na+]>>Cl.N1=C2C(=NO1)C=C(C=C2)CCN2CCC1(CC2)OC2=C(C(C1)=O)C=C(C=C2)NS(=O)(=O)C
Br[CH2:19][CH2:20][c:21]1[cH:22][cH:23][c:24]2[n:25][o:26][n:27][c:28]2[cH:29]1.[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[C:12](=[O:13])[CH2:14][C:15]1([CH2:16][CH2:17][NH:18][CH2:30][CH2:31]1)[O:32]2>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[C:12](=[O:...
BrCCc1ccc2nonc2c1.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc4nonc4c3)CC1)O2
null
null
C(C)O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
fcc4a915ce374c4aab389e812dfb69762e7b96d1b9afab3cb3150e76db46ecf6
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1CC2(CCN(CCc3ccc4nonc4c3)CC2)Oc2ccccc21
Br-[CH2;D2;+0:1]-[C:2]-[c:3].[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8]>>[C:4]-[C:5]-[N;H0;D3;+0:6](-[CH2;D2;+0:1]-[C:2]-[c:3])-[C:7]-[C:8]
41.2
[{"value": 41.0, "product": "Cl.N1=C2C(=NO1)C=C(C=C2)CCN2CCC1(CC2)OC2=C(C(C1)=O)C=C(C=C2)NS(=O)(=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 41.2, "product": "Cl.N1=C2C(=NO1)C=C(C=C2)CCN2CCC1(CC2)OC2=C(C(C1)=O)C=C(C=C2)NS(=O)(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A suspension of 5-(2-bromoethyl)benzofurazan (0.39 g, 1.72 mmol), 3,4-dihydro-6-methanesulfonamidospiro[(2H)-1-benzopyran-2,4'-piperidine]-4-one hydrochloride (0.24 g, 0.69 mmol) and sodium bicarbonate (0.21 g, 2.55 mmol) in ethanol (13.2 ml) was heated at reflux temperature for 24 hr. Solvent evaporation and chromatog...
10.6084/m9.figshare.5104873.v1
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Primary halide.Secondary amine
Tertiary amine
c1ccc2c(c1)CCC1(CCNCC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1ccc2nonc2c1
HBr
C(C)O
null
null
BrCCc1ccc2nonc2c1.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2>C(C)O>CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc4nonc4c3)CC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-947d6841260549d3b54d67fb4a7179a9
CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.O=[N+]([O-])c1ccc(CBr)cc1>>CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(Cc3ccc([N+](=O)[O-])cc3)CC1)O2
CO.C(Cl)(Cl)Cl.[N+](=O)([O-])C1=CC=C(CBr)C=C1.C(C)(=O)NC=1C=CC2=C(C(CC3(CCNCC3)O2)=O)C1.C(C)(C)N(CC)C(C)C>>C(C)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CC3=CC=C(C=C3)[N+](=O)[O-])O2)=O)C1
[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]2[c:9]([cH:10]1)[C:11](=[O:12])[CH2:13][C:14]1([CH2:15][CH2:16][NH:17][CH2:28][CH2:29]1)[O:30]2.Br[CH2:18][c:19]1[cH:20][cH:21][c:22]([N+:23](=[O:24])[O-:25])[cH:26][cH:27]1>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]2[c:9]([cH:10]1)[C:11](=[O:12])[CH2:13][C:14]1(...
CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.O=[N+]([O-])c1ccc(CBr)cc1
CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(Cc3ccc([N+](=O)[O-])cc3)CC1)O2
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
fcc4a915ce374c4aab389e812dfb69762e7b96d1b9afab3cb3150e76db46ecf6
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1CC2(CCN(Cc3ccccc3)CC2)Oc2ccccc21
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]>>[C:5]-[C:6]-[N;H0;D3;+0:7](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:8]-[C:9]
59.6
[{"value": 59.0, "product": "C(C)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CC3=CC=C(C=C3)[N+](=O)[O-])O2)=O)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 59.6, "product": "C(C)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CC3=CC=C(C=C3)[N+](=O)[O-])O2)=O)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 4-nitrobenzyl bromide (0.73 g, 3.4 mmol), 3,4-dihydro-6-acetamidospiro[(2H)-benzopyran-2,4'-piperidine]-4-one (0.94 g, 3.4 mmol) and diisopropylethylamine (0.61 ml, 3.5 mmol) in dimethylformamide (15 ml) was stirred at room temperature for 3 hr. The reaction mixture was then concentrated under reduced pre...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
c1ccc2c(c1)CCC1(CCNCC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1ccccc1
HBr
CN(C=O)C
null
null
CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.O=[N+]([O-])c1ccc(CBr)cc1>CN(C=O)C>CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(Cc3ccc([N+](=O)[O-])cc3)CC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-9b03d7f6f2964e45a150ed7ab18aa7c8
CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(Cc3ccc([N+](=O)[O-])cc3)CC1)O2>>CC(=O)Nc1ccc2c(c1)CCC1(CCN(Cc3ccc(N)cc3)CC1)O2
C(C)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CC3=CC=C(C=C3)[N+](=O)[O-])O2)=O)C1.C([O-])(O)=O.[Na+].[OH-].[Na+]>>C(C)(=O)NC=1C=CC2=C(CCC3(CCN(CC3)CC3=CC=C(C=C3)N)O2)C1
O=[C:11]1[c:9]2[c:8]([cH:7][cH:6][c:5]([NH:4][C:2]([CH3:1])=[O:3])[cH:10]2)[O:27][C:13]2([CH2:12]1)[CH2:14][CH2:15][N:16]([CH2:17][c:18]1[cH:19][cH:20][c:21]([N+:22](=O)[O-])[cH:23][cH:24]1)[CH2:25][CH2:26]2>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]2[c:9]([cH:10]1)[CH2:11][CH2:12][C:13]1([CH2:14][CH2:15][N:16]...
CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(Cc3ccc([N+](=O)[O-])cc3)CC1)O2
CC(=O)Nc1ccc2c(c1)CCC1(CCN(Cc3ccc(N)cc3)CC1)O2
null
[Cl-].[Ti+3].[Cl-].[Cl-]
C(C)(=O)O
Reduction
OtherReaction
8985ded34c0bf81299f9e2b3f91a3f7ce647b50d45f1547836f6a2340637be4a
3c5c7ef2400d5d2a996d2d09cdefbec5aec3351f5fc8a14a05fd6968a0753f9f
c1ccc(CN2CCC3(CCc4ccccc4O3)CC2)cc1
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[#8:4]-[c:5]:[c:6]-1:[c:7].O=[N+;H0;D3:8](-[O-])-[c:9](:[c:10]):[c:11]>>[NH2;D1;+0:8]-[c:9](:[c:10]):[c:11].[c:7]:[c:6]1:[c:5]-[#8:4]-[C:3]-[C:2]-[CH2;D2;+0:1]-1
82.1
[{"value": 82.1, "product": "C(C)(=O)NC=1C=CC2=C(CCC3(CCN(CC3)CC3=CC=C(C=C3)N)O2)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 3,4-dihydro-6-acetamido-1'-(4-nitrobenzyl)spiro[(2H)-1-benzopyran-2,4'-piperidine]-4-one (0.58 g, 1.4 mmol) in acetic acid (6.4 ml) was added titanium (III) chloride (15% wt. in 20-30% wt. hydrochloric acid, 7 ml) dropwise. The reaction mixture was stirred at room temperature for 1 hr, cooled to 0° C. ...
10.6084/m9.figshare.5104873.v1
null
Ketone.Nitro group
Primary amine
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1ccccc1
Other
[Cl-].[Ti+3].[Cl-].[Cl-].C(C)(=O)O
null
1
CC(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(Cc3ccc([N+](=O)[O-])cc3)CC1)O2>[Cl-].[Ti+3].[Cl-].[Cl-].C(C)(=O)O>CC(=O)Nc1ccc2c(c1)CCC1(CCN(Cc3ccc(N)cc3)CC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-876d879d6ec744549debf35e4e67563d
CC(=O)Nc1ccc2c(c1)CCC1(CCN(Cc3ccc(N)cc3)CC1)O2>>Nc1ccc(CN2CCC3(CC2)CC(=O)c2cc(N)ccc2O3)cc1
C(C)(=O)NC=1C=CC2=C(CCC3(CCN(CC3)CC3=CC=C(C=C3)N)O2)C1.Cl.[OH-].[Na+]>>NC=1C=CC2=C(C(CC3(CCN(CC3)CC3=CC=C(C=C3)N)O2)=O)C1
CC(=[O:15])[NH:19][c:18]1[cH:17][c:16]2[c:22]([cH:21][cH:20]1)[O:23][C:10]1([CH2:9][CH2:8][N:7]([CH2:6][c:5]3[cH:4][cH:3][c:2]([NH2:1])[cH:25][cH:24]3)[CH2:12][CH2:11]1)[CH2:13][CH2:14]2>>[NH2:1][c:2]1[cH:3][cH:4][c:5]([CH2:6][N:7]2[CH2:8][CH2:9][C:10]3([CH2:11][CH2:12]2)[CH2:13][C:14](=[O:15])[c:16]2[cH:17][c:18]([NH2...
CC(=O)Nc1ccc2c(c1)CCC1(CCN(Cc3ccc(N)cc3)CC1)O2
Nc1ccc(CN2CCC3(CC2)CC(=O)c2cc(N)ccc2O3)cc1
null
null
CO
Miscellaneous
OtherReaction
01a04d52e078c4be97f885a20207f56a20ea0668290cc0e817af8c04fa5216b2
66f3156bebb43aa378bf50af0944e3de9570ac5cc9f6d0d57adc66597251de20
O=C1CC2(CCN(Cc3ccccc3)CC2)Oc2ccccc21
C-C(=[O;H0;D1;+0:1])-[NH;D2;+0:2]-[c:3](:[c:4]):[c:5]:[c:6]1:[c:7]-[#8:8]-[C:9]-[C:10]-[CH2;D2;+0:11]-1>>[NH2;D1;+0:2]-[c:3](:[c:4]):[c:5]:[c:6]1:[c:7]-[#8:8]-[C:9]-[C:10]-[C;H0;D3;+0:11]-1=[O;H0;D1;+0:1]
88
[{"value": 88.0, "product": "NC=1C=CC2=C(C(CC3(CCN(CC3)CC3=CC=C(C=C3)N)O2)=O)C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3,4-dihydro-6-acetamido-1'-(4-aminobenzyl)spiro[(2H)-1-benzopyran-2,4'-piperidine] (136 mg, 0.36 mmol) and hydrochloric acid (6N solution, 13.6 ml) in methanol (13.6 ml) was heated at reflux temperature for 1 hr. The reaction mixture was cooled to 0° C. and basified with 20% sodium hydroxide solution. Ext...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
Ketone.Primary amine
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccccc1.c1ccc2c(c1)CCC1(CC[NH]CC1)O2
Other
CO
null
null
CC(=O)Nc1ccc2c(c1)CCC1(CCN(Cc3ccc(N)cc3)CC1)O2>CO>Nc1ccc(CN2CCC3(CC2)CC(=O)c2cc(N)ccc2O3)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-3e41f9accd6644a589cc4ef9c8e97232
COC(=O)c1ccc(-n2ccnc2)cc1>>OCc1ccc(-n2ccnc2)cc1
COC(C1=CC=C(C=C1)N1C=NC=C1)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3].C1CCOC1>>OCC1=CC=C(C=C1)N1C=NC=C1
CO[C:2](=[O:1])[c:3]1[cH:4][cH:5][c:6](-[n:7]2[cH:8][cH:9][n:10][cH:11]2)[cH:12][cH:13]1>>[OH:1][CH2:2][c:3]1[cH:4][cH:5][c:6](-[n:7]2[cH:8][cH:9][n:10][cH:11]2)[cH:12][cH:13]1
COC(=O)c1ccc(-n2ccnc2)cc1
OCc1ccc(-n2ccnc2)cc1
null
null
C1CCOC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(-n2ccnc2)cc1
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3](:[c:4]):[c:5]>>[OH;D1;+0:2]-[CH2;D2;+0:1]-[c:3](:[c:4]):[c:5]
98
[{"value": 98.0, "product": "OCC1=CC=C(C=C1)N1C=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
To a mixture of 4-(1H-imidazol-1-yl)benzoic acid methyl ester (prepared as described in U.S. Pat. No. 4,804,662) (1.5 g) in THF (25 ml) at -15° C. was added a solution of 1M LAH/THF (10.4) ml). The mixture was stirred for 1/2 hour and allowed to warm to room temperature. The reaction was quenched by addition of water (...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccccc1.c1c[nH]cn1
Other
C1CCOC1
null
0.5
COC(=O)c1ccc(-n2ccnc2)cc1>C1CCOC1>OCc1ccc(-n2ccnc2)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-21549f1abd034e7fa819e5d32eb716a4
CSCCN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2>>CS(=O)(=O)CCN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2
CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CCSC)O2)=O)C1.OOS(=O)[O-].[K+].O.C(=O)(O)[O-].[Na+]>>CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CCS(=O)(=O)C)O2)=O)C1
[CH3:1][S:2][CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][C:10]2([CH2:11][CH2:12]1)[CH2:13][C:14](=[O:15])[c:16]1[cH:17][c:18]([NH:19][S:20]([CH3:21])(=[O:22])=[O:23])[cH:24][cH:25][c:26]1[O:27]2>>[CH3:1][S:2](=[O:3])(=[O:4])[CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][C:10]2([CH2:11][CH2:12]1)[CH2:13][C:14](=[O:15])[c:16]1[cH:17][c:18]([N...
CSCCN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2
CS(=O)(=O)CCN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2
null
null
CO
Oxidation
OtherReaction
20dd6d48007b4fe7cd760226f21413eb5e71e6468db112596c2e7ea4858c8ac1
5cedc1bf0f43f21d78a249521ecfcec19fc5ac4895c41eed0e84f0c2618149fa
O=C1CC2(CCNCC2)Oc2ccccc21
[C:1]-[C:2]-[S;H0;D2;+0:3]-[C;D1;H3:4]>>[C:1]-[C:2]-[S;H0;D4;+0:3](-[C;D1;H3:4])(=[O;D1;H0:5])=[O;D1;H0:6]
44.6
[{"value": 44.6, "product": "CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CCS(=O)(=O)C)O2)=O)C1", "details": "PERCENTYIELD", "is_desired": false}]
25
CELSIUS
2
HOUR
A solution of 6-methanesulfonamido-3,4-dihydro-1'-(2-methylthioethyl)spiro[(2H)-1-benzopyran-2,4'-piperidine]-4-one (0.335 g, 0.871 mmol) in 15 mL of methanol was treated dropwise with a solution of Oxone® (0.803 g, 1.31 mmol) in 15 mL of water. The resulting mixture was stirred at 25° C. for 2 hours. The reaction mixt...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfone
null
null
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
null
CO
25
2
CSCCN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2>CO>CS(=O)(=O)CCN1CCC2(CC1)CC(=O)c1cc(NS(C)(=O)=O)ccc1O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-525f17d072ad44f5b9d585107ba4daf9
CC(=O)Cl.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc(N)cc3)CC1)O2>>CC(=O)Nc1ccc(CCN2CCC3(CC2)CC(=O)c2cc(NS(C)(=O)=O)ccc2O3)cc1
CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CCC3=CC=C(C=C3)N)O2)=O)C1.N1=CC=CC=C1.C(C)(=O)Cl>>CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CCC3=CC=C(C=C3)NC(C)=O)O2)=O)C1
Cl[C:2]([CH3:1])=[O:3].[NH2:4][c:5]1[cH:6][cH:7][c:8]([CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][C:14]3([CH2:15][CH2:16]2)[CH2:17][C:18](=[O:19])[c:20]2[cH:21][c:22]([NH:23][S:24]([CH3:25])(=[O:26])=[O:27])[cH:28][cH:29][c:30]2[O:31]3)[cH:32][cH:33]1>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]([CH2:9][CH2:10][N:11]2...
CC(=O)Cl.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc(N)cc3)CC1)O2
CC(=O)Nc1ccc(CCN2CCC3(CC2)CC(=O)c2cc(NS(C)(=O)=O)ccc2O3)cc1
null
null
C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
O=C1CC2(CCN(CCc3ccccc3)CC2)Oc2ccccc21
Cl-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[NH;D2;+0:4]-[c:5](:[c:6]):[c:7]
18
[{"value": 18.0, "product": "CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CCC3=CC=C(C=C3)NC(C)=O)O2)=O)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 17.7, "product": "CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CCC3=CC=C(C=C3)NC(C)=O)O2)=O)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
A suspension of 6-methanesulfonamido-3,4-dihydro-1'-(2-(4-aminophenyl)ethyl)-spiro[(2H)-1-benzopyran-2,4'-piperidine]-4-one (0.50 g, 1.2 mmol), and pyridine (0.09 mL, 1.2 mmol) in 25 mL of methylene chloride was cooled in an ice bath and treated dropwise with acetyl chloride (0.09 mL, 1.2 mmol). The mixture was stirred...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccc2c(c1)CCC1(CC[NH]CC1)O2
HCl
C(Cl)Cl
0
2
CC(=O)Cl.CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc(N)cc3)CC1)O2>C(Cl)Cl>CC(=O)Nc1ccc(CCN2CCC3(CC2)CC(=O)c2cc(NS(C)(=O)=O)ccc2O3)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ef0eae7f82d04b7abdea25f31eba98a9
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.ClCCc1ccc(Cl)nc1>>CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc(Cl)nc3)CC1)O2
ClC1=CC=C(C=N1)CC(=O)O.Cl.CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCNCC3)O2)=O)C1.Cl.ClC1=NC=C(C=C1)CCCl.S(=O)(Cl)Cl.Cl.ClC1=NC=C(C=C1)CCCl>>CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCN(CC3)CCC=3C=CC(=NC3)Cl)O2)=O)C1
[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[C:12](=[O:13])[CH2:14][C:15]1([CH2:16][CH2:17][NH:18][CH2:28][CH2:29]1)[O:30]2.Cl[CH2:19][CH2:20][c:21]1[cH:22][cH:23][c:24]([Cl:25])[n:26][cH:27]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[C:12](=[O:13])[CH2:14...
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.ClCCc1ccc(Cl)nc1
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc(Cl)nc3)CC1)O2
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
fcc4a915ce374c4aab389e812dfb69762e7b96d1b9afab3cb3150e76db46ecf6
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1CC2(CCN(CCc3cccnc3)CC2)Oc2ccccc21
Cl-[CH2;D2;+0:1]-[C:2]-[c:3]:[c:4]:[#7;a:5].[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[#7;a:5]:[c:4]:[c:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:8](-[C:7]-[C:6])-[C:9]-[C:10]
null
[]
null
null
null
null
The title compound was prepared from 3,4-dihydro-6-methanesulfonamidospiro[(2H)-1-benzopyran-2,4'-piperidine]-4-one hydrochloride and 2-chloro-5-chloroethylpyridine hydrochloride by a procedure analogous to that described in Example 92, Step B. [The 2-chloro-5-chloroethylpyridine hydrochloride used in this reaction was...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
c1ccc2c(c1)CCC1(CCNCC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1ccncc1
HCl
null
null
null
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.ClCCc1ccc(Cl)nc1>>CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc(Cl)nc3)CC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-e8fb55e1737e4827b7e769d1e042ed5c
BrCCBr.C=C(C)n1c(=O)[nH]c2ccccc21>>C=C(C)n1c(=O)n(CCBr)c2ccccc21
C(=C)(C)N1C(NC2=C1C=CC=C2)=O.BrCCBr.[H-].[Na+]>>C(=C)(C)N1C(N(C2=C1C=CC=C2)CCBr)=O
Br[CH2:8][CH2:9][Br:10].[CH2:1]=[C:2]([CH3:3])[n:4]1[c:5](=[O:6])[nH:7][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]12>>[CH2:1]=[C:2]([CH3:3])[n:4]1[c:5](=[O:6])[n:7]([CH2:8][CH2:9][Br:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]12
BrCCBr.C=C(C)n1c(=O)[nH]c2ccccc21
C=C(C)n1c(=O)n(CCBr)c2ccccc21
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
798c3cd6443cfe7f029ed03c4760cf76103b5f272c5de707760a27469f565eca
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=c1[nH]c2ccccc2[nH]1
Br-[CH2;D2;+0:1]-[C:2]-[Br;D1;H0:3].[C;D1;H2:4]=[C:5]-[#7;a:6]1:[c:7](:[c:8]):[c:9](:[c:10]):[nH;D2;+0:11]:[c:12]:1=[O;D1;H0:13]>>[Br;D1;H0:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:11]1:[c:9](:[c:10]):[c:7](:[c:8]):[#7;a:6](-[C:5]=[C;D1;H2:4]):[c:12]:1=[O;D1;H0:13]
null
[]
null
null
null
null
1-Isopropenylbenzimidazolone (J. Davol, J. Chem. Soc., 1960, 308) was alkylated with 1,2-dibromoethane using sodium hydride in DMF. The product was purified by chromatography and crystallization from cyclohexane to give 1-isopropenyl-3-(2-bromoethyl)benzimidazolone. Conditions: See reaction.notes.procedure_details. Wor...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1ccc2[nH]cnc2c1
c1nc2ccccc2[nH]1
c1nc2ccccc2[nH]1
HBr
CN(C)C=O
null
null
BrCCBr.C=C(C)n1c(=O)[nH]c2ccccc21>CN(C)C=O>C=C(C)n1c(=O)n(CCBr)c2ccccc21
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-318a0d649152403aa70213f1e775d186
N#Cc1ccc(CCO)cc1>>NCc1ccc(CCO)cc1
C(#N)C1=CC=C(CCO)C=C1.Cl>>OCCC1=CC=C(CN)C=C1
[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][OH:9])[cH:10][cH:11]1>>[NH2:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][OH:9])[cH:10][cH:11]1
N#Cc1ccc(CCO)cc1
NCc1ccc(CCO)cc1
null
[Pd]
C(C)O
Reduction
Reduction of nitrile to amine
65bec2d9f430701d30dc9fcbe1c5418f3dfa174d67be035c50edfc71895dc9c7
e8d1bc928b94bd4f5bf4b23363ce8f88b1ce7d146ba93829e7b8ad8dbe0007a7
c1ccccc1
[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[NH2;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]
null
[]
null
null
null
null
A solution of 0.74 g (0.005 mol) of p-cyanophenethyl alcohol in 50 ml of ethanol containing 10 ml of concentrated hydrochloric acid was hydrogenated at 30 psi using 0.1 g 5% Pd/C for 72 hours. The catalyst was removed by filtration and the solvent was removed under reduced pressure. Conditions: See reaction.notes.proce...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
c1ccccc1
null
[Pd].C(C)O
null
null
N#Cc1ccc(CCO)cc1>[Pd].C(C)O>NCc1ccc(CCO)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-9c1c7be5dc37482b9254a181f9161fc1
CN.CSC(=NCc1ccc(CCO)cc1)NC#N>>CNC(=NCc1ccc(CCO)cc1)NC#N
C(#N)NC(SC)=NCC1=CC=C(C=C1)CCO.CN>>C(#N)NC(=NCC1=CC=C(C=C1)CCO)NC
[CH3:1][NH2:2].CS[C:3](=[N:4][CH2:5][c:6]1[cH:7][cH:8][c:9]([CH2:10][CH2:11][OH:12])[cH:13][cH:14]1)[NH:15][C:16]#[N:17]>>[CH3:1][NH:2][C:3](=[N:4][CH2:5][c:6]1[cH:7][cH:8][c:9]([CH2:10][CH2:11][OH:12])[cH:13][cH:14]1)[NH:15][C:16]#[N:17]
CN.CSC(=NCc1ccc(CCO)cc1)NC#N
CNC(=NCc1ccc(CCO)cc1)NC#N
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
2ebe33ae3b7bb48bd968f9b830d6d3b488b85670dea18c3fe37a1f418e787d67
88e0224d19b2dce8f9987d52554afb32090d36ff7ee19e89dc5bf66d30974ec4
c1ccccc1
C-S-[C;H0;D3;+0:1](-[#7:2]-[C:3]#[N;D1;H0:4])=[#7:5]-[C:6].[C;D1;H3:7]-[NH2;D1;+0:8]>>[C:6]-[#7:5]=[C;H0;D3;+0:1](-[#7:2]-[C:3]#[N;D1;H0:4])-[NH;D2;+0:8]-[C;D1;H3:7]
null
[]
null
null
null
null
A solution of 0.42 g (0.00168 mol) of N-cyano-N'-[4-(2-hydroxyethyl)benzyl]-S-methylisothiourea in 50 ml of methanol and 10 g of methylamine was stirred at room temperature overnight. Evaporation of the solvent gave the title compound. Conditions: See reaction.notes.procedure_details. Workup: Evaporation of the solvent
10.6084/m9.figshare.5104873.v1
null
Primary amine.Monosulfide
Secondary amine
null
null
c1ccccc1
Other
CO
null
null
CN.CSC(=NCc1ccc(CCO)cc1)NC#N>CO>CNC(=NCc1ccc(CCO)cc1)NC#N
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-5316fdb95ac1472fad8e43ff4c6050cf
COc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.Cn1c(Cl)cc(=O)n(C)c1=O>>COc1ccc2c(c1)C(=O)CC1(CCN(c3cc(=O)n(C)c(=O)n3C)CC1)O2
Cl.COC=1C=CC2=C(C(CC3(CCNCC3)O2)=O)C1.ClC1=CC(N(C(N1C)=O)C)=O.C([O-])(O)=O.[Na+]>>COC=1C=CC2=C(C(CC3(CCN(CC3)C3=CC(N(C(N3C)=O)C)=O)O2)=O)C1
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[C:9](=[O:10])[CH2:11][C:12]1([CH2:13][CH2:14][NH:15][CH2:26][CH2:27]1)[O:28]2.Cl[c:16]1[cH:17][c:18](=[O:19])[n:20]([CH3:21])[c:22](=[O:23])[n:24]1[CH3:25]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[C:9](=[O:10])[CH2:11][C:12]1([CH2:13][CH2:14][N:15]([c:16]3[c...
COc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.Cn1c(Cl)cc(=O)n(C)c1=O
COc1ccc2c(c1)C(=O)CC1(CCN(c3cc(=O)n(C)c(=O)n3C)CC1)O2
null
null
C(C)#N
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
bc34618442e5983c32b958a7ba036a5956ffdb399bcfda57c8d7a1117867fc26
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
O=C1CC2(CCN(c3cc(=O)[nH]c(=O)[nH]3)CC2)Oc2ccccc21
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3](=[O;D1;H0:4]):[#7;a:5](-[C;D1;H3:6]):[c:7](=[O;D1;H0:8]):[#7;a:9]:1-[C;D1;H3:10].[C:11]-[C:12]-[NH;D2;+0:13]-[C:14]-[C:15]>>[C:11]-[C:12]-[N;H0;D3;+0:13](-[c;H0;D3;+0:1]1:[c:2]:[c:3](=[O;D1;H0:4]):[#7;a:5](-[C;D1;H3:6]):[c:7](=[O;D1;H0:8]):[#7;a:9]:1-[C;D1;H3:10])-[C:14]-[C:15]
61
[{"value": 61.0, "product": "COC=1C=CC2=C(C(CC3(CCN(CC3)C3=CC(N(C(N3C)=O)C)=O)O2)=O)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 61.0, "product": "COC=1C=CC2=C(C(CC3(CCN(CC3)C3=CC(N(C(N3C)=O)C)=O)O2)=O)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3,4-dihydro-6-methoxyspiro[(2H)-1-benzopyran-2,4'-piperidin]-4-one hydrochloride (0.568 g, 2 mmol), 6-chloro-1,3-dimethylpyrimidine-2,4-(1H,3H)-dione (0.349 g, 2 mmol) and sodium bicarbonate (0.42 g, 5 mmol) in acetonitrile was heated at reflux for 42 hours. After cooling, the reaction mixture was concent...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
c1ccc2c(c1)CCC1(CCNCC1)O2.c1cncnc1
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1cncnc1
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1cncnc1
HCl
C(C)#N
null
null
COc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.Cn1c(Cl)cc(=O)n(C)c1=O>C(C)#N>COc1ccc2c(c1)C(=O)CC1(CCN(c3cc(=O)n(C)c(=O)n3C)CC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-88c9f74d06f8450f9794988fded824ed
COc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.Cn1c(Cl)cc(=O)n(C)c1=O.NCCCl>>COc1ccc2c(c1)C(=O)CC1(CCN(NCCc3cc(=O)n(C)c(=O)n3C)CC1)O2
COC=1C=CC2=C(C(CC3(CCNCC3)O2)=O)C1.C([O-])(O)=O.[Na+].ClC1=CC(N(C(N1C)=O)C)=O.C([O-])(O)=O.[Na+].Cl.ClCCN>>COC=1C=CC2=C(C(CC3(CCN(CC3)NCCC3=CC(N(C(N3C)=O)C)=O)O2)=O)C1
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[C:9](=[O:10])[CH2:11][C:12]1([CH2:13][CH2:14][NH:15][CH2:29][CH2:30]1)[O:31]2.Cl[c:19]1[cH:20][c:21](=[O:22])[n:23]([CH3:24])[c:25](=[O:26])[n:27]1[CH3:28].Cl[CH2:18][CH2:17][NH2:16]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[C:9](=[O:10])[CH2:11][C:12]1([CH2:...
COc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.Cn1c(Cl)cc(=O)n(C)c1=O.NCCCl
COc1ccc2c(c1)C(=O)CC1(CCN(NCCc3cc(=O)n(C)c(=O)n3C)CC1)O2
null
null
C(C)#N
C-C Coupling
OtherReaction
e5d14b9a1390e93fd473cc0623468fae4ee720b2637de5e9ac381352607b0271
18003c40afa0ae7056d4af614852fee10a5b33bbd4fc564f4ecabd7cb824e747
O=C1CC2(CCN(NCCc3cc(=O)[nH]c(=O)[nH]3)CC2)Oc2ccccc21
Cl-[CH2;D2;+0:1]-[C:2]-[NH2;D1;+0:3].Cl-[c;H0;D3;+0:4]1:[c:5]:[c:6](=[O;D1;H0:7]):[#7;a:8](-[C;D1;H3:9]):[c:10](=[O;D1;H0:11]):[#7;a:12]:1-[C;D1;H3:13].[C:14]-[C:15]-[NH;D2;+0:16]-[C:17]-[C:18]>>[C:14]-[C:15]-[N;H0;D3;+0:16](-[NH;D2;+0:3]-[C:2]-[CH2;D2;+0:1]-[c;H0;D3;+0:4]1:[c:5]:[c:6](=[O;D1;H0:7]):[#7;a:8](-[C;D1;H3:...
10.5
[{"value": 10.5, "product": "COC=1C=CC2=C(C(CC3(CCN(CC3)NCCC3=CC(N(C(N3C)=O)C)=O)O2)=O)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 10.5, "product": "COC=1C=CC2=C(C(CC3(CCN(CC3)NCCC3=CC(N(C(N3C)=O)C)=O)O2)=O)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
28
HOUR
A suspension of 3,4-dihydro-6-methoxyspiro[(2H)-1-benzopyran-2,4'-piperidin]-4-one (0.284 g, 1 mmol) and sodium bicarbonate (0.42 g, 5 mmol) in acetonitrile was heated at reflux for 1 hour, 2-chloro ethylamine hydrochloride (0.116 g, 1 mmol) was added the solution was heated at reflux for 17 hours, 6-chloro-1,3-dimethy...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary halide.Primary amine.Secondary amine
Hydrazine
c1ccc2c(c1)CCC1(CCNCC1)O2.c1cncnc1
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1cncnc1
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1cncnc1
HCl
C(C)#N
null
28
COc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.Cn1c(Cl)cc(=O)n(C)c1=O.NCCCl>C(C)#N>COc1ccc2c(c1)C(=O)CC1(CCN(NCCc3cc(=O)n(C)c(=O)n3C)CC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-7ff27640a0d54d469b56503d444125ed
CC(=O)Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1[N+](=O)[O-]>>Nc1ccc(CCN2CCC(=O)CC2)cc1[N+](=O)[O-]
C(C)(=O)NC1=C(C=C(C=C1)CCN1CCC2(OCCO2)CC1)[N+](=O)[O-].C([O-])([O-])=O.[Na+].[Na+].[OH-].[Na+]>>NC1=C(C=C(C=C1)CCN1CCC(CC1)=O)[N+](=O)[O-]
CC(=O)[NH:1][c:2]1[cH:3][cH:4][c:5]([CH2:6][CH2:7][N:8]2[CH2:9][CH2:10][C:11]3(OCC[O:12]3)[CH2:13][CH2:14]2)[cH:15][c:16]1[N+:17](=[O:18])[O-:19]>>[NH2:1][c:2]1[cH:3][cH:4][c:5]([CH2:6][CH2:7][N:8]2[CH2:9][CH2:10][C:11](=[O:12])[CH2:13][CH2:14]2)[cH:15][c:16]1[N+:17](=[O:18])[O-:19]
CC(=O)Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1[N+](=O)[O-]
Nc1ccc(CCN2CCC(=O)CC2)cc1[N+](=O)[O-]
null
null
Cl.O
Miscellaneous
OtherReaction
176e3c936f8b0228a9f0ca46976463d0d009d1179afb166ac4c2da9f24278672
b81fbae8c1fcf1836374d8300cfb4cb18a278d33ac9b4c50c799b24d221cbea0
O=C1CCN(CCc2ccccc2)CC1
C-C(=O)-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4].C1-C-[O;H0;D2;+0:5]-[C;H0;D4;+0:6]2(-O-1)-[C:7]-[C:8]-[#7:9]-[C:10]-[C:11]-2>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;H0;D1;+0:5]=[C;H0;D3;+0:6]1-[C:7]-[C:8]-[#7:9]-[C:10]-[C:11]-1
100
[{"value": 100.0, "product": "NC1=C(C=C(C=C1)CCN1CCC(CC1)=O)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A suspension of 5.24 g (15.0 mmol) of 1-(8-[2-(4-acetamido-3-nitrophenyl)ethyl]-1,4-dioxa-8-azaspiro[4.5]decane in 30 mL 2N hydrochloric acid was heated at reflux for 1.5 hours. The cooled mixture was basified (pH 9-10) with saturated sodium carbonate solution and 10N sodium hydroxide, diluted with 100 ml water, and ex...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Secondary amide
Ketone.Primary amine
C1CC2(CC[NH]1)OCCO2
C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1
HO-
Cl.O
null
null
CC(=O)Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1[N+](=O)[O-]>Cl.O>Nc1ccc(CCN2CCC(=O)CC2)cc1[N+](=O)[O-]
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-15723b5096154a8997b8fde29ebb3e38
N#Cc1ccc(CCO)nc1>>C=Cc1ccc(C#N)cn1
C(#N)C=1C=CC(=NC1)CCO.O.C1(=CC=C(C=C1)S(=O)(=O)O)C.C([O-])(O)=O.[Na+]>>C(#N)C=1C=CC(=NC1)C=C
O[CH2:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([C:7]#[N:8])[cH:9][n:10]1>>[CH2:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([C:7]#[N:8])[cH:9][n:10]1
N#Cc1ccc(CCO)nc1
C=Cc1ccc(C#N)cn1
null
null
C1(=CC=CC=C1)C
Functional Group Interconversion
OtherReaction
567ff9e729a2d16a3e456243eaa6fea906fc7f4a844968338133cf6b5d71906c
962c102d7e14de3254b057440327853861d9d966484d1838cbc59a673a23337d
c1ccncc1
O-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[#7;a:5]:[c:6]>>[CH2;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[#7;a:5]:[c:6]
36.3
[{"value": 36.0, "product": "C(#N)C=1C=CC(=NC1)C=C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 36.3, "product": "C(#N)C=1C=CC(=NC1)C=C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 0.163 g (1.1 mmol) 5-cyano-2-(2-hydroxyethyl)pyridine and 0.029 g (0.15 mmol) p-toluenesulfonic acid hydrate in 10 mL toluene was heated to reflux for five hours in a flask equipped with a Dean-Stark trap. The cooled mixture was neutralized with 5 mL saturated sodium bicarbonate solution and extracted with...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Vinyl
null
null
c1ccncc1
HO-
C1(=CC=CC=C1)C
null
null
N#Cc1ccc(CCO)nc1>C1(=CC=CC=C1)C>C=Cc1ccc(C#N)cn1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-1b3fc702fdbd4fa5893859a012326d24
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.CS(=O)(=O)OCCc1ccc2ncsc2c1>>CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc4ncsc4c3)CC1)O2
Cl.CS(=O)(=O)NC=1C=CC2=C(C(CC3(CCNCC3)O2)=O)C1.C([O-])(O)=O.[Na+].CS(=O)(=O)OCCC1=CC2=C(N=CS2)C=C1.[I-].[K+]>>Cl.S1C=NC2=C1C=C(C=C2)CCN2CCC1(CC2)OC2=C(C(C1)=O)C=C(C=C2)NS(=O)(=O)C
[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[C:12](=[O:13])[CH2:14][C:15]1([CH2:16][CH2:17][NH:18][CH2:30][CH2:31]1)[O:32]2.CS(=O)(=O)O[CH2:19][CH2:20][c:21]1[cH:22][cH:23][c:24]2[n:25][cH:26][s:27][c:28]2[cH:29]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]2[c:10]([cH:11]1)[...
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.CS(=O)(=O)OCCc1ccc2ncsc2c1
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc4ncsc4c3)CC1)O2
null
null
C(C)#N
Heteroatom Alkylation and Arylation
Alkylation of amines
cf82d2a38f125ca8c9949e8e8f3aeaad2fce343be85d05de0088847feeb0d203
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=C1CC2(CCN(CCc3ccc4ncsc4c3)CC2)Oc2ccccc21
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[c:3].[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8]>>[C:4]-[C:5]-[N;H0;D3;+0:6](-[CH2;D2;+0:1]-[C:2]-[c:3])-[C:7]-[C:8]
48
[{"value": 48.0, "product": "Cl.S1C=NC2=C1C=C(C=C2)CCN2CCC1(CC2)OC2=C(C(C1)=O)C=C(C=C2)NS(=O)(=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 47.8, "product": "Cl.S1C=NC2=C1C=C(C=C2)CCN2CCC1(CC2)OC2=C(C(C1)=O)C=C(C=C2)NS(=O)(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
In a manner similar to that described in Example 92, Step B a mixture of 3,4-dihydro-6-methanesulfonamido-spiro[(2H)-1-benzopyran-2,4'-piperidine]-4-one hydrochloride (0.146 g, 0.42 mmol), sodium bicarbonate (0.143 g, 1.70 mmol), 6-benzothiazolylethyl methanesulfonate (0.108 g, 0.42 mmol), potassium iodide (0.070 g, 0....
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
c1ccc2c(c1)CCC1(CCNCC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2
c1ccc2c(c1)CCC1(CC[NH]CC1)O2.c1ccc2scnc2c1
MsOH.HO-
C(C)#N
null
null
CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCNCC1)O2.CS(=O)(=O)OCCc1ccc2ncsc2c1>C(C)#N>CS(=O)(=O)Nc1ccc2c(c1)C(=O)CC1(CCN(CCc3ccc4ncsc4c3)CC1)O2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-10f0b3d1151e4129a36d8f920eff1d36
CSCc1ccc(O)c(C(C)=O)c1.[O-][I+3]([O-])([O-])[O-]>>CC(=O)c1cc(CS(C)=O)ccc1O
OC1=C(C=C(C=C1)CSC)C(C)=O.I(=O)(=O)(=O)[O-].[Na+]>>OC1=C(C=C(C=C1)CS(=O)C)C(C)=O
[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([CH2:7][S:8][CH3:9])[cH:11][cH:12][c:13]1[OH:14].[O-][I+3]([O-])([O-])[O-:10]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([CH2:7][S:8]([CH3:9])=[O:10])[cH:11][cH:12][c:13]1[OH:14]
CSCc1ccc(O)c(C(C)=O)c1.[O-][I+3]([O-])([O-])[O-]
CC(=O)c1cc(CS(C)=O)ccc1O
null
null
O.CO
Oxidation
OtherReaction
9edfaf6d72a81452ea8e3a1cdcb10a58409fff36608e97019e7273998b3d5373
f5f6bb6ca76a2267cd589767b4d67e7a17ab1ac383eeb6143dcd5d92e00e1b6a
c1ccccc1
[C;D1;H3:1]-[S;H0;D2;+0:2]-[C:3]-[c:4].[O-;H0;D1:5]-[I+3](-[O-])(-[O-])-[O-]>>[C;D1;H3:1]-[S;H0;D3;+0:2](=[O;H0;D1;+0:5])-[C:3]-[c:4]
60
[{"value": 60.0, "product": "OC1=C(C=C(C=C1)CS(=O)C)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 59.5, "product": "OC1=C(C=C(C=C1)CS(=O)C)C(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a solution of 2'-hydroxy-5'-(methylthiomethyl)acetophenone (2.20 g, 11.0 mmol) in 70 mL MeOH cooled in an ice bath was added a solution of sodium metaperiodate (2.49 g, 12.1 mmol) in 115 mL water. The resulting cloudy mixture was stirred two hours with cooling then partially concentrated in vacuo to remove methanol....
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfoxide
null
null
c1ccccc1
I-
O.CO
null
2
CSCc1ccc(O)c(C(C)=O)c1.[O-][I+3]([O-])([O-])[O-]>O.CO>CC(=O)c1cc(CS(C)=O)ccc1O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-88eceac4d7b14e2ba62b61092830aadb
CSCc1ccc(O)c(C(C)=O)c1>>CC(=O)c1cc(CS(C)(=O)=O)ccc1O
OC1=C(C=C(C=C1)CSC)C(C)=O.CO.OOS(=O)[O-].[K+]>>OC1=C(C=C(C=C1)CS(=O)(=O)C)C(C)=O
[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([CH2:7][S:8][CH3:9])[cH:12][cH:13][c:14]1[OH:15]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([CH2:7][S:8]([CH3:9])(=[O:10])=[O:11])[cH:12][cH:13][c:14]1[OH:15]
CSCc1ccc(O)c(C(C)=O)c1
CC(=O)c1cc(CS(C)(=O)=O)ccc1O
null
null
O
Oxidation
OtherReaction
20dd6d48007b4fe7cd760226f21413eb5e71e6468db112596c2e7ea4858c8ac1
5cedc1bf0f43f21d78a249521ecfcec19fc5ac4895c41eed0e84f0c2618149fa
c1ccccc1
[C;D1;H3:1]-[S;H0;D2;+0:2]-[C:3]-[c:4]>>[C;D1;H3:1]-[S;H0;D4;+0:2](=[O;D1;H0:5])(=[O;D1;H0:6])-[C:3]-[c:4]
null
[]
null
null
2
HOUR
To a solution of 2'-hydroxy-5'-(methylthiomethyl)acetophenone (2.20 g, 11.0 mmol) in 88 mL methanol cooled in an ice bath was added a solution of OXONE (commercial potassium peroxymonosulfate mixture, Aldrich Chemical Co.)(20.28 g, 33.0 mmol) in 88 mL water. The mixture was stirred two hours with cooling then partially...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfone
null
null
c1ccccc1
null
O
null
2
CSCc1ccc(O)c(C(C)=O)c1>O>CC(=O)c1cc(CS(C)(=O)=O)ccc1O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-58e4f6ee25724c079c75ffc776570d5f
CC(=O)c1cc(CCl)ccc1O.CS(N)(=O)=O>>CC(=O)c1cc(CNS(C)(=O)=O)ccc1O
CS(=O)(=O)N.[H-].[Na+].ClCC=1C=CC(=C(C1)C(C)=O)O.Cl>>OC1=C(C=C(C=C1)CNS(=O)(=O)C)C(C)=O
Cl[CH2:7][c:6]1[cH:5][c:4]([C:2]([CH3:1])=[O:3])[c:15]([OH:16])[cH:14][cH:13]1.[NH2:8][S:9]([CH3:10])(=[O:11])=[O:12]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([CH2:7][NH:8][S:9]([CH3:10])(=[O:11])=[O:12])[cH:13][cH:14][c:15]1[OH:16]
CC(=O)c1cc(CCl)ccc1O.CS(N)(=O)=O
CC(=O)c1cc(CNS(C)(=O)=O)ccc1O
null
null
CS(=O)C
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
4b9697564fc265ba44ddc16e54c39ac37f4ae3b83733e16918a5dac2d316c1f0
3fe6b65897247a134b277f2a2d6b241ddeabbd8a2611ba8aad88f24ab3c1380a
c1ccccc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C;D1;H3:5]-[#16:6](-[NH2;D1;+0:7])(=[O;D1;H0:8])=[O;D1;H0:9]>>[C;D1;H3:5]-[#16:6](=[O;D1;H0:8])(=[O;D1;H0:9])-[NH;D2;+0:7]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
12.3
[{"value": 12.0, "product": "OC1=C(C=C(C=C1)CNS(=O)(=O)C)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 12.3, "product": "OC1=C(C=C(C=C1)CNS(=O)(=O)C)C(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a mixture of sodium hydride (60% dispersion in mineral oil, 1.60 g, 40.0 mmol) in 25 mL DMSO under Argon was added dropwise a solution of methanesulfonamide (3.80 g, 40.0 mmol) in 10 mL DMSO. The resulting mixture was stirred 30 minutes and a solution of 5'-(chloromethyl)-2'-hydroxyacetophenone (3.69 g, 20.0 mmol) i...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Primary halide
Sulfonamide
null
null
c1ccccc1
HCl
CS(=O)C
null
0.5
CC(=O)c1cc(CCl)ccc1O.CS(N)(=O)=O>CS(=O)C>CC(=O)c1cc(CNS(C)(=O)=O)ccc1O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-34d79860ad584cf385dcffca66a922f8
CC(=O)c1cc(CCl)ccc1O.COCCO>>COCCOCc1ccc(O)c(C(C)=O)c1
ClCC=1C=CC(=C(C1)C(C)=O)O.C([O-])([O-])=O.[K+].[K+].COCCO>>OC1=C(C=C(C=C1)COCCOC)C(C)=O
Cl[CH2:6][c:7]1[cH:8][cH:9][c:10]([OH:11])[c:12]([C:13]([CH3:14])=[O:15])[cH:16]1.[CH3:1][O:2][CH2:3][CH2:4][OH:5]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][c:7]1[cH:8][cH:9][c:10]([OH:11])[c:12]([C:13]([CH3:14])=[O:15])[cH:16]1
CC(=O)c1cc(CCl)ccc1O.COCCO
COCCOCc1ccc(O)c(C(C)=O)c1
null
null
C(Cl)(Cl)Cl
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
dd3f9c60e1f90d961a7c01d970ae213561355ee1451f276a3b04696e4b6fae5c
46a6e883cf919b4006e69abfdfd883f458f55c08b3200960c6a5b57c4139fbca
c1ccccc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]-[OH;D1;+0:7]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
18
[{"value": 18.0, "product": "OC1=C(C=C(C=C1)COCCOC)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 17.8, "product": "OC1=C(C=C(C=C1)COCCOC)C(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A mixture of 5'-(chloromethyl)-2'-hydroxyacetophenone (1.85 g, 10.0 mmol), potassium carbonate (1.38, 10.0 mmol), 2-methoxyethanol (0.91 g, 12.0 mmol) and 10 mL chloroform was stirred 24 hours, filtered, and the filtrate concentrated in vacuo to give a residue. The residue was purified by flash chromatography eluting w...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary alcohol
Ether
null
null
c1ccccc1
HCl
C(Cl)(Cl)Cl
null
24
CC(=O)c1cc(CCl)ccc1O.COCCO>C(Cl)(Cl)Cl>COCCOCc1ccc(O)c(C(C)=O)c1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-08e1b55496fe4cbebd59e0dd24ef1b14
CC(=O)c1cc(CCl)ccc1O.O=C1CCCN1>>CC(=O)c1cc(CN2CCCC2=O)ccc1O
N1C(CCC1)=O.[H-].[Na+].ClCC=1C=CC(=C(C1)C(C)=O)O.Cl>>C(C)(=O)C=1C=C(C=CC1O)CN1C(CCC1)=O
Cl[CH2:7][c:6]1[cH:5][c:4]([C:2]([CH3:1])=[O:3])[c:16]([OH:17])[cH:15][cH:14]1.[NH:8]1[CH2:9][CH2:10][CH2:11][C:12]1=[O:13]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([CH2:7][N:8]2[CH2:9][CH2:10][CH2:11][C:12]2=[O:13])[cH:14][cH:15][c:16]1[OH:17]
CC(=O)c1cc(CCl)ccc1O.O=C1CCCN1
CC(=O)c1cc(CN2CCCC2=O)ccc1O
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
f5f217f17d493fffc808e7019c66db8bb20f63ec70b29db349ba715e196bdaf0
4a6c1e88c9e8bed487b746792f88d478ff36cc235f9a217d4632e6babdebdc9a
O=C1CCCN1Cc1ccccc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C:6]1-[C:7]-[C:8]-[C:9]-[NH;D2;+0:10]-1>>[O;D1;H0:5]=[C:6]1-[C:7]-[C:8]-[C:9]-[N;H0;D3;+0:10]-1-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
82.3
[{"value": 82.0, "product": "C(C)(=O)C=1C=C(C=CC1O)CN1C(CCC1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.3, "product": "C(C)(=O)C=1C=C(C=CC1O)CN1C(CCC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a suspension of sodium hydride (60% dispersion in mineral oil, 0.80 g, 20.0 mmol) in 15 mL dry dimethylformamide under argon, cooled in an ice-bath was added dropwise a solution of 2-pyrrolidinone (1.70 g, 20.0 mmol) in 5 mL dimethylformamide. The ice-bath was removed, the mixture was stirred 30 minutes, and a solut...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amide
Tertiary amide
C1CCNC1
C1CC[NH]C1
c1ccccc1.C1CC[NH]C1
HCl
CN(C=O)C
null
0.5
CC(=O)c1cc(CCl)ccc1O.O=C1CCCN1>CN(C=O)C>CC(=O)c1cc(CN2CCCC2=O)ccc1O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-dc93e323f5dd4fdea38a1dcf99643bf1
CC(=O)c1cc(CCl)ccc1O.O=C1NCCN1>>CC(=O)c1cc(CN2CCNC2=O)ccc1O
[H-].[Na+].ClCC=1C=CC(=C(C1)C(C)=O)O.N1C(NCC1)=O>>C(C)(=O)C=1C=C(C=CC1O)CN1C(NCC1)=O
Cl[CH2:7][c:6]1[cH:5][c:4]([C:2]([CH3:1])=[O:3])[c:16]([OH:17])[cH:15][cH:14]1.[NH:8]1[CH2:9][CH2:10][NH:11][C:12]1=[O:13]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([CH2:7][N:8]2[CH2:9][CH2:10][NH:11][C:12]2=[O:13])[cH:14][cH:15][c:16]1[OH:17]
CC(=O)c1cc(CCl)ccc1O.O=C1NCCN1
CC(=O)c1cc(CN2CCNC2=O)ccc1O
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
9e337ae0278d976da02093acd3b0ff1860ee7514970cc3a05771bc3416d56448
9068cdf0ef9ef7510e3ed725979384397a613e011a5abb0653feb8d5b2408c81
O=C1NCCN1Cc1ccccc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C:6]1-[#7:7]-[C:8]-[C:9]-[NH;D2;+0:10]-1>>[O;D1;H0:5]=[C:6]1-[#7:7]-[C:8]-[C:9]-[N;H0;D3;+0:10]-1-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
43.1
[{"value": 43.0, "product": "C(C)(=O)C=1C=C(C=CC1O)CN1C(NCC1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 43.1, "product": "C(C)(=O)C=1C=C(C=CC1O)CN1C(NCC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a suspension of sodium hydride (60% dispersion in mineral oil, 0.80 g, 20.0 mmol) in 15 mL dry dimethylformamide under argon, cooled in an ice-bath was added dropwise a solution of 2-imidazolidone (1.72 g, 20.0 mmol) in 5 mL dimethylformamide. The ice bath was removed, the mixture was stirred 30 minutes and a soluti...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Urea
Urea
C1CNCN1
C1CNC[NH]1
c1ccccc1.C1CNC[NH]1
HCl
CN(C=O)C
null
0.5
CC(=O)c1cc(CCl)ccc1O.O=C1NCCN1>CN(C=O)C>CC(=O)c1cc(CN2CCNC2=O)ccc1O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-310c58e7bbc14872a5a2fd0b11d6f844
C1CC2(CCN1)OCCO2.O=[N+]([O-])c1ccc(CCBr)cc1>>O=[N+]([O-])c1ccc(CCC2COC3(CCNCC3)O2)cc1
O1CCOC12CCNCC2.C([O-])([O-])=O.[K+].[K+].[N+](=O)([O-])C1=CC=C(C=C1)CCBr>>[N+](=O)([O-])C1=CC=C(C=C1)CCC1OC2(OC1)CCNCC2
[CH2:10]1[CH2:11][O:12][C:13]2([CH2:14][CH2:15][NH:16][CH2:17][CH2:18]2)[O:19]1.Br[CH2:9][CH2:8][c:7]1[cH:6][cH:5][c:4]([N+:2](=[O:1])[O-:3])[cH:21][cH:20]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([CH2:8][CH2:9][CH:10]2[CH2:11][O:12][C:13]3([CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)[O:19]2)[cH:20][cH:21]1
C1CC2(CCN1)OCCO2.O=[N+]([O-])c1ccc(CCBr)cc1
O=[N+]([O-])c1ccc(CCC2COC3(CCNCC3)O2)cc1
null
null
C(C)#N
C-C Coupling
OtherReaction
c66afc65e24cb62c882739e3a122ebd7ace4fc27b44a2c5954ad220497e3a037
2c1c1647472d7e3cff37f0f3aad955b760f0ad2f8b7aa7e7825b1c0344bab3bb
c1ccc(CCC2COC3(CCNCC3)O2)cc1
Br-[CH2;D2;+0:1]-[C:2]-[c:3].[#8:4]1-[C:5]-[CH2;D2;+0:6]-[#8:7]-[C:8]-1>>[c:3]-[C:2]-[CH2;D2;+0:1]-[CH;D3;+0:6]1-[#8:7]-[C:8]-[#8:4]-[C:5]-1
null
[]
0
CELSIUS
10
MINUTE
1,4-Dioxa-8-azaspiro[4.5]-decane (18.62 g, 130 mmoles) in 50 mL of acetonitrile was stirred under argon and treated with anhydrous potassium carbonate (27.60 g, 200 mmoles). The mixture was cooled to 0° C. and 2-(4-nitrophenyl)ethylbromide (23.01 g, 100 mmoles) was added in one portion. After 10 minutes, the ice bath w...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether
Ether
C1CC2(CCN1)OCCO2
C1CC2(CCN1)OCCO2
c1ccccc1.C1CC2(CCN1)OCCO2
HBr
C(C)#N
0
0.166667
C1CC2(CCN1)OCCO2.O=[N+]([O-])c1ccc(CCBr)cc1>C(C)#N>O=[N+]([O-])c1ccc(CCC2COC3(CCNCC3)O2)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a2c1a5bf1f6c453393f3e3747eac03ce
CC(=O)OC(C)=O.CC(=O)OC(C)=O.Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1.O=[N+]([O-])O>>CC(=O)Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1[N+](=O)[O-].CC(=O)O
C(C)(=O)OC(C)=O.NC1=CC=C(C=C1)CCN1CCC2(OCCO2)CC1.[N+](=O)(O)[O-].C(C)(=O)OC(C)=O>>C(C)(=O)O.N(C(=O)C)C1=C(C=C(C=C1)CCN1CCC2(OCCO2)CC1)[N+](=O)[O-]
CC(=O)[O:29][C:27]([CH3:26])=[O:28].CC(=O)O[C:2]([CH3:1])=[O:3].[NH2:4][c:5]1[cH:6][cH:7][c:8]([CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][C:14]3([CH2:15][CH2:16]2)[O:17][CH2:18][CH2:19][O:20]3)[cH:21][cH:22]1.O[N+:23](=[O:24])[O-:25]>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]([CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][...
CC(=O)OC(C)=O.CC(=O)OC(C)=O.Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1.O=[N+]([O-])O
CC(=O)Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1[N+](=O)[O-].CC(=O)O
null
null
[Cl-].[Na+].O.C(Cl)Cl
Acylation
OtherReaction
3fe925e789c7af32c97d8e327c658191abf45cdab6265c77681e8bb2b1ae9e60
c70ebc153fece6477741db56cc6e65053f7fa07f58324ca5bad12977626bef94
c1ccc(CCN2CCC3(CC2)OCCO3)cc1
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].C-C(=O)-[O;H0;D2;+0:4]-[C:5](-[C;D1;H3:6])=[O;D1;H0:7].O-[N+;H0;D3:8](-[O;-;D1;H0:9])=[O;D1;H0:10].[NH2;D1;+0:11]-[c:12](:[c:13]):[cH;D2;+0:14]:[c:15]:[c:16]>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[NH;D2;+0:11]-[c:12](:[c:13]):[c;H0;D3;+0:14](-[N+;H0;D3:8](-[O;-;D1;...
89
[{"value": 89.0, "product": "C(C)(=O)O.N(C(=O)C)C1=C(C=C(C=C1)CCN1CCC2(OCCO2)CC1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}]
-5
CELSIUS
18
HOUR
A mechanically stirred solution of N(2-(4-aminophenyl)ethyl)-1,4-dioxa-8-azaspiro[4.5]-decane in methylene chloride (400 mL) cooled to -5° C. under an argon atmosphere was treated dropwise with acetic anhydride (58.8 mL, 622 mmoles). The reaction was allowed to reach room temperature and was stirred for 18 hr. After th...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Anhydride.Nitrate.Primary amine
Carboxylic acid.Nitro group.Secondary amide
c1ccccc1
c1ccccc1
c1ccccc1.C1CC2(CC[NH]1)OCCO2
HO-
[Cl-].[Na+].O.C(Cl)Cl
-5
18
CC(=O)OC(C)=O.CC(=O)OC(C)=O.Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1.O=[N+]([O-])O>[Cl-].[Na+].O.C(Cl)Cl>CC(=O)Nc1ccc(CCN2CCC3(CC2)OCCO3)cc1[N+](=O)[O-].CC(=O)O