dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
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-c3a75813d0b24864aa4f7cd526efd6aa
ord-1904c867b1b84d10aefb06cd7dec1eac
CCOCC.O=C(Cl)CCCCl.Oc1cccc(F)c1.Oc1ccccc1>>O=C(CCCCl)c1ccc(F)cc1O.O=C(CCCCl)c1ccccc1O
B(F)(F)F.CCOCC.FC=1C=C(C=CC1)O.C1(=CC=CC=C1)O.ClCCCC(=O)Cl>>ClCCCC(=O)C1=C(C=C(C=C1)F)O.ClCCCC(=O)C1=C(C=CC=C1)O
[O:15]([CH2:16][CH3:17])[CH2:19][CH3:18].[O:1]=[C:2]([CH2:3][CH2:4][CH2:5][Cl:6])[Cl:20].[cH:7]1[cH:8][cH:9][c:10]([F:11])[cH:12][c:13]1[OH:14].[cH:21]1[cH:22][cH:23][cH:24][cH:25][c:26]1[OH:27]>>[O:1]=[C:2]([CH2:3][CH2:4][CH2:5][Cl:6])[c:7]1[cH:8][cH:9][c:10]([F:11])[cH:12][c:13]1[OH:14].[O:15]=[C:16]([CH2:17][CH2:18]...
CCOCC.O=C(Cl)CCCCl.Oc1cccc(F)c1.Oc1ccccc1
O=C(CCCCl)c1ccc(F)cc1O.O=C(CCCCl)c1ccccc1O
null
null
null
C-C Coupling
OtherReaction
f6e3f5fae6ba9aa012e548b2c7e7796d55f302a3eb278dd6c088c97d5fcc073e
a8db79155e5f746b7dfdd411e413dcf17b0d00a9bf013adc4221557f79162a3f
c1ccccc1.c1ccccc1
[CH3;D1;+0:1]-[CH2;D2;+0:2]-[O;H0;D2;+0:3]-[CH2;D2;+0:4]-[CH3;D1;+0:5].[C:6]-[C:7]-[C;H0;D3;+0:8](-[Cl;H0;D1;+0:9])=[O;D1;H0:10].[O;D1;H1:11]-[c:12](:[c:13]):[cH;D2;+0:14]:[c:15]:[c:16].[O;D1;H1:17]-[c:18](:[c:19]):[cH;D2;+0:20]:[c:21]:[c:22]>>[C:6]-[C:7]-[C;H0;D3;+0:8](=[O;D1;H0:10])-[c;H0;D3;+0:14](:[c:15]:[c:16]):[c...
null
[]
130
CELSIUS
18
HOUR
To a cold boron trifluoride etherate (280 mmol) solution was added 3-fluorophenol or phenol (89 mmol) and 4-chlorobutyryl chloride (178 mmol). The resulting solution was stirred at 130° C. for 18 hours. The reaction mixture was cooled and poured into ice water (100 mL). After stirring for 10 minutes, the water mixture ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether
Primary halide.Ketone.Ketone
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
null
null
130
18
CCOCC.O=C(Cl)CCCCl.Oc1cccc(F)c1.Oc1ccccc1>>O=C(CCCCl)c1ccc(F)cc1O.O=C(CCCCl)c1ccccc1O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1c9db1114b854c7eb84e757a71c7335f
CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12.Fc1ccc2c(CCCCl)noc2c1>>CN1CCN2c3c(cccc31)[C@@H]1CN(CCCc3noc4cc(F)ccc34)CC[C@@H]12.Cl
ClCCCC1=NOC2=C1C=CC(=C2)F.CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1.N>>Cl.FC1=CC2=C(C(=NO2)CCCN2C[C@@H]3[C@@H](N4CCN(C=5C=CC=C3C45)C)CC2)C=C1
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[C@@H:12]1[CH2:13][NH:14][CH2:28][CH2:29][C@H:30]21.[CH2:15]([CH2:16][CH2:17][c:18]1[n:19][o:20][c:21]2[cH:22][c:23]([F:24])[cH:25][cH:26][c:27]12)[Cl:31]>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[C@@H:12]1[CH2:13]...
CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12.Fc1ccc2c(CCCCl)noc2c1
CN1CCN2c3c(cccc31)[C@@H]1CN(CCCc3noc4cc(F)ccc34)CC[C@@H]12.Cl
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
e632fd65463eb262ac3c07c304635f39a39b141a1af7e45d1ba4958b16cbff9a
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1cc2c3c(c1)[C@@H]1CN(CCCc4noc5ccccc45)CC[C@@H]1N3CCN2
[C:1]-[C:2]-[CH2;D2;+0:3]-[Cl;H0;D1;+0:4].[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]>>[C:5]-[C:6]-[N;H0;D3;+0:7](-[CH2;D2;+0:3]-[C:2]-[C:1])-[C:8]-[C:9].[ClH;D0;+0:4]
null
[]
null
null
null
null
The title compound was prepared from addition of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole from Step D and (6bR,10aS)-3-methyl-2,3,6b,7,8,9,10,10a-octahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline following General procedure A, Example 197. 1H NMR (300 MHz, CDCl3) δ 7.63 (dd, J=8.8 Hz, 4.7 Hz, 1H), 7.20–7....
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1ccc2oncc2c1.c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
null
null
null
null
CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12.Fc1ccc2c(CCCCl)noc2c1>>CN1CCN2c3c(cccc31)[C@@H]1CN(CCCc3noc4cc(F)ccc34)CC[C@@H]12.Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-df231b2eefe7403fa727fe476aa6064d
CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12.ClCCCc1noc2ccccc12>>CN1CCN2c3c(cccc31)[C@@H]1CN(CCCc3noc4ccccc34)CC[C@@H]12.Cl
ClCCCC1=NOC2=C1C=CC=C2.CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1.N>>Cl.O1N=C(C2=C1C=CC=C2)CCCN2C[C@@H]1[C@@H](N3CCN(C=4C=CC=C1C34)C)CC2
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[C@@H:12]1[CH2:13][NH:14][CH2:27][CH2:28][C@H:29]21.[CH2:15]([CH2:16][CH2:17][c:18]1[n:19][o:20][c:21]2[cH:22][cH:23][cH:24][cH:25][c:26]12)[Cl:30]>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[C@@H:12]1[CH2:13][N:14](...
CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12.ClCCCc1noc2ccccc12
CN1CCN2c3c(cccc31)[C@@H]1CN(CCCc3noc4ccccc34)CC[C@@H]12.Cl
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
e632fd65463eb262ac3c07c304635f39a39b141a1af7e45d1ba4958b16cbff9a
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1cc2c3c(c1)[C@@H]1CN(CCCc4noc5ccccc45)CC[C@@H]1N3CCN2
[C:1]-[C:2]-[CH2;D2;+0:3]-[Cl;H0;D1;+0:4].[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]>>[C:5]-[C:6]-[N;H0;D3;+0:7](-[CH2;D2;+0:3]-[C:2]-[C:1])-[C:8]-[C:9].[ClH;D0;+0:4]
null
[]
null
null
null
null
The title compound was prepared from addition 3-(3-chloropropyl)-1,2-benzisoxazole from Step D Example 22 and (6bR,10aS)-3-methyl-2,3,6b,7,8,9,10,10a-octahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline following the General procedure A of Example 197. 1H NMR (300 MHz, CDCl3) δ 7.59–7.62 (m, 1H), 7.46–7.50 (m, 2H...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1ccc2oncc2c1.c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
null
null
null
null
CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12.ClCCCc1noc2ccccc12>>CN1CCN2c3c(cccc31)[C@@H]1CN(CCCc3noc4ccccc34)CC[C@@H]12.Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d00d1a250cf64390bc55c24d83d3a652
CCOC(=O)N1CCc2c(c3cccc4c3n2CC(=O)N4)C1>>CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3
[OH-].[Na+].C(#N)[BH3-].[Na+].O=C1NC=2C=CC=C3C2N(C1)C1=C3CN(CC1)C(=O)OCC.[OH-].[NH4+]>>O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][c:9]2[c:10]([c:12]3[cH:13][cH:14][cH:15][c:16]4[c:17]3[n:18]2[CH2:19][C:20](=[O:21])[NH:22]4)[CH2:11]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][C@H:9]2[C@@H:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:17]1[N:18]2[CH2:19][C:20](=[O:21])[NH:22]3
CCOC(=O)N1CCc2c(c3cccc4c3n2CC(=O)N4)C1
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3
null
null
FC(C(=O)O)(F)F
Reduction
OtherReaction
6fe5078fa337973e230c6466957c05e6e5e019f7173f54dc2b3cce93e1834287
3f9bd1254c561719832bd71149feb4e99c5764db1feb47bf9fbdfb1c414d602b
O=C1CN2c3c(cccc3[C@@H]3CNCC[C@@H]32)N1
[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[c;H0;D3;+0:6]2:[c:7](:[c:8]):[c:9]3:[c:10]-[#7:11]-[C:12](=[O;D1;H0:13])-[C:14]-[n;H0;D3;+0:15]:3:[c;H0;D3;+0:16]:2-[C:17]-[C:18]-1>>[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[C@@H;D3;+0:6]2-[C@H;D3;+0:16](-[C:17]-[C:18]-1)-[N;H0;D3;+0:15]1-[C:14]-[C:12](=[O;D1;H0:13])-[#7:11]-[...
90.3
[{"value": 90.0, "product": "O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.3, "product": "O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Sodium cyanoborohydride (4.0 g, 65 mmol) was added, in small portions, to a vigorously stirred solution of ethyl 2,3,9,10-tetrahydro-2-oxo-1H-pyrido[3′,4′:4,5]-pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (11.97 g, 40 mmol) in trifluoroacetic acid (125 mL) cooled in an ice-water bath, under nitrogen. After the additi...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amine
c1cc2c3c(c1)c1c(n3CCN2)CC[NH]C1
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
null
FC(C(=O)O)(F)F
null
0.5
CCOC(=O)N1CCc2c(c3cccc4c3n2CC(=O)N4)C1>FC(C(=O)O)(F)F>CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-09747b86a1ae4216958fb9948c11d0d9
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI>>CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3C
[H-].[Na+].O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC.IC>>CN1C(CN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)C(=O)OCC)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][C@H:9]2[C@@H:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:17]1[N:18]2[CH2:19][C:20](=[O:21])[NH:22]3.I[CH3:23]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][C@H:9]2[C@@H:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:17]1[N:18]2[CH2:19][C:20](=[O:...
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3C
null
null
CCCCCC.CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
980d07b89e1a95150d6f8a4b1bb819c09ac2db99776f72555e02c19625afb4f5
0a16658309ac5595448433dd7ef49294830b145345df0b202ccd54727262e629
O=C1CN2c3c(cccc3[C@@H]3CNCC[C@@H]32)N1
I-[CH3;D1;+0:1].[O;D1;H0:2]=[C:3]1-[C:4]-[#7:5]-[c:6]:[c:7](:[c:8])-[NH;D2;+0:9]-1>>[CH3;D1;+0:1]-[N;H0;D3;+0:9]1-[C:3](=[O;D1;H0:2])-[C:4]-[#7:5]-[c:6]:[c:7]-1:[c:8]
87
[{"value": 87.0, "product": "CN1C(CN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)C(=O)OCC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.9, "product": "CN1C(CN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)C(=O)OCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
Sodium hydride (900 mg of 60% dispersion in oil; 22.5 mmol) was washed with hexane, and suspended in anhydrous dimethylformamide (5 mL). The suspension was added to a stirred solution of ethyl (6bR,10aS)-2-oxo-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (6.02 g, 20 mmol)...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
Tertiary amide
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
HI
CCCCCC.CN(C=O)C
null
1
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI>CCCCCC.CN(C=O)C>CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4408fc5ded764b36931f251d7cf317fd
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3C>>CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CCN3C
B.CN1C(CN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)C(=O)OCC)=O.Cl>>CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)C(=O)OCC
O=[C:20]1[CH2:19][N:18]2[C@H:9]3[CH2:8][CH2:7][N:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:11][C@H:10]3[c:12]3[cH:13][cH:14][cH:15][c:16]([c:17]32)[N:21]1[CH3:22]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][C@H:9]2[C@@H:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:17]1[N:18]2[CH2:19][CH2:20][N:21]3[CH3:...
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3C
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CCN3C
null
null
O1CCCC1
Reduction
Reduction of tertiary amides to amines
b85edbb5fb9a189d3d5456aab7a3bf994122238d91275bcbace6c7a052dc91bc
c8f3c617792f7a4fae96b8a97dc0ce23461ab85d8a738fe6caacff776ef51ffa
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CCN2
O=[C;H0;D3;+0:1]1-[C:2]-[#7:3](-[C:4])-[c:5]:[c:6]-[#7:7]-1-[C;D1;H3:8]>>[C:4]-[#7:3]1-[C:2]-[CH2;D2;+0:1]-[#7:7](-[C;D1;H3:8])-[c:6]:[c:5]-1
93
[{"value": 93.0, "product": "CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.9, "product": "CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of borane in tetrahydrofuran (1M, 33 mL, 33 mmol) was added dropwise to a stirred solution of ethyl (6bR,10aS)-3-methyl-2-oxo-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (5.24 g, 16.6 mmol) in anhydrous tetrahydrofuran (25 mL) under nitrogen. After the additio...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
null
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
Other
O1CCCC1
null
null
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3C>O1CCCC1>CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CCN3C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-46d7f2d51615421183cda533e5cd96d7
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CCN3C>>CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
[OH-].[K+].CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)C(=O)OCC>>CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1
CCOC(=O)[N:14]1[CH2:13][C@H:12]2[c:7]3[c:6]4[c:11]([cH:10][cH:9][cH:8]3)[N:2]([CH3:1])[CH2:3][CH2:4][N:5]4[C@H:17]2[CH2:16][CH2:15]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[C@@H:12]1[CH2:13][NH:14][CH2:15][CH2:16][C@H:17]21
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CCN3C
CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
null
null
C(CCC)O
Reduction
Hydrogenolysis of tertiary amines
64340f7d0b350a19bf30b154f1ce71f378bd544e8fb5c5b6b78431eb1ca1b0d3
20c36f41eeb07c3ba4437b51ba72e8ff3c22d0b27e7197b0e9af3127f331149f
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CCN2
C-C-O-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]
95.1
[{"value": 95.0, "product": "CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.1, "product": "CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Powdered potassium hydroxide (10.0 g) was added to a stirred solution of ethyl (6bR,10aS)-3-methyl-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (4.52 g, 15.0 mmol) in warm 1-butanol (50 mL) and the resulting mixture was heated under reflux for 5 h. It was then evaporated ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether
Secondary amine
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
HO-
C(CCC)O
null
null
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CCN3C>C(CCC)O>CN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8357a7c9abfa492eb4945ce6cff6b78e
CCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3>>CCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC.C(C)I>>C(C)N1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1
I[CH2:2][CH3:1].CCOC(=O)[N:15]1[CH2:14][C@H:13]2[c:8]3[c:7]4[c:12]([cH:11][cH:10][cH:9]3)[NH:3][C:4](=O)[CH2:5][N:6]4[C@H:18]2[CH2:17][CH2:16]1>>[CH3:1][CH2:2][N:3]1[CH2:4][CH2:5][N:6]2[c:7]3[c:8]([cH:9][cH:10][cH:11][c:12]31)[C@@H:13]1[CH2:14][NH:15][CH2:16][CH2:17][C@H:18]21
CCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3
CCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
260fe71a473b60bc6699adc87a714c283b8e75d0d15e5c63eedaf0773c2c0554
5fa8b50dba8178d1bbd9e21cc84d8eae82649eda60ef87b4318bbafd818aae11
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CCN2
C-C-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4](-[C:5]-[C:6]-1)-[#7:7]1-[C:8]-[C;H0;D3;+0:9](=O)-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]-1.I-[CH2;D2;+0:14]-[C;D1;H3:15]>>[C;D1;H3:15]-[CH2;D2;+0:14]-[N;H0;D3;+0:10]1-[CH2;D2;+0:9]-[C:8]-[#7:7](-[c:13]:[c:11]-1:[c:12])-[C:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:6]-[C:5]-1
null
[]
null
null
null
null
Utilizing the material from Example 255 Step A, the title compound was prepared in analogous fashion using ethyl iodide as the alkyl halide and following the procedure of Step B–D of Example 255, as a light brown amorphous solid. 1H NMR (CDCl3, 300 MHz) δ 1.15 (t, 3H), 1.70–2.01 (m, 3H), 2.65–2.70 (t, J=9.6 Hz, 3H), 2....
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carbamic ester.Ether.Secondary amide
Secondary amine.Tertiary amine
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
HI
null
null
null
CCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3>>CCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d2c035a66a65479c9eed8a8bc8c5ee6f
CCCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3>>CCCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC.C(CC)I>>C(CC)N1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1
I[CH2:3][CH2:2][CH3:1].CCOC(=O)[N:16]1[CH2:15][C@H:14]2[c:9]3[c:8]4[c:13]([cH:12][cH:11][cH:10]3)[NH:4][C:5](=O)[CH2:6][N:7]4[C@H:19]2[CH2:18][CH2:17]1>>[CH3:1][CH2:2][CH2:3][N:4]1[CH2:5][CH2:6][N:7]2[c:8]3[c:9]([cH:10][cH:11][cH:12][c:13]31)[C@@H:14]1[CH2:15][NH:16][CH2:17][CH2:18][C@H:19]21
CCCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3
CCCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
260fe71a473b60bc6699adc87a714c283b8e75d0d15e5c63eedaf0773c2c0554
5fa8b50dba8178d1bbd9e21cc84d8eae82649eda60ef87b4318bbafd818aae11
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CCN2
C-C-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4](-[C:5]-[C:6]-1)-[#7:7]1-[C:8]-[C;H0;D3;+0:9](=O)-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]-1.I-[CH2;D2;+0:14]-[C:15]-[C;D1;H3:16]>>[C;D1;H3:16]-[C:15]-[CH2;D2;+0:14]-[N;H0;D3;+0:10]1-[CH2;D2;+0:9]-[C:8]-[#7:7](-[c:13]:[c:11]-1:[c:12])-[C:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:6]-[C:5]-...
null
[]
null
null
null
null
Utilizing the material from Example 255 Step A, the title compound was prepared in analogous fashion using propyl iodide as the alkyl halide and following the procedure of Step B–D of Example 255, as an amorphous tan solid. 1H NMR (CDCl3, 300 MHz) δ 0.94 (t, 2H), 1.40–2.01 (m, 6H), 2.65–2.70 (t, J=9.6 Hz, 2H), 2.70–2.9...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carbamic ester.Ether.Secondary amide
Secondary amine.Tertiary amine
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
HI
null
null
null
CCCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3>>CCCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a0db3e26d47a4482b8294d3c5d4b1751
CC(C)I.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3>>CC(C)N1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC.C(C)(C)I>>C(C)(C)N1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1
I[CH:2]([CH3:1])[CH3:3].CCOC(=O)[N:16]1[CH2:15][C@H:14]2[c:9]3[c:8]4[c:13]([cH:12][cH:11][cH:10]3)[NH:4][C:5](=O)[CH2:6][N:7]4[C@H:19]2[CH2:18][CH2:17]1>>[CH3:1][CH:2]([CH3:3])[N:4]1[CH2:5][CH2:6][N:7]2[c:8]3[c:9]([cH:10][cH:11][cH:12][c:13]31)[C@@H:14]1[CH2:15][NH:16][CH2:17][CH2:18][C@H:19]21
CC(C)I.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3
CC(C)N1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
51aba3152c403e3828f480df1c24fd00e01a93b9bef445a427db2a590eb0513e
4ab0d2871f7ad18e2c7831a2fc2049eb9f2385b09b03e2f3a97a520e61bae71b
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CCN2
C-C-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4](-[C:5]-[C:6]-1)-[#7:7]1-[C:8]-[C;H0;D3;+0:9](=O)-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]-1.I-[CH;D3;+0:14](-[C;D1;H3:15])-[C;D1;H3:16]>>[C;D1;H3:15]-[CH;D3;+0:14](-[C;D1;H3:16])-[N;H0;D3;+0:10]1-[CH2;D2;+0:9]-[C:8]-[#7:7](-[c:13]:[c:11]-1:[c:12])-[C:4]1-[C:3]-[C:2]-[NH;D2;+0:1...
null
[]
null
null
null
null
Utilizing the material from Example 255 Step A, the title compound was prepared in analogous fashion using isopropyl iodide as the alkyl halide and following the procedure of Step B–D of Example 255, as a viscous brown liquid. 1H NMR (CDCl3, 300 MHz) δ 1.18 (d, 6H), 1.60–1.67 (m, 1H), 1.71–1.94 (m, 2H), 2.63–2.75 (m, 2...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Carbamic ester.Ether.Secondary amide
Secondary amine.Tertiary amine
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
HI
null
null
null
CC(C)I.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3>>CC(C)N1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-acdd2e919cd744928b60cc08194548e8
CCCCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3>>CCCCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC.C(CCC)I>>C(CCC)N1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1
I[CH2:4][CH2:3][CH2:2][CH3:1].CCOC(=O)[N:17]1[CH2:16][C@H:15]2[c:10]3[c:9]4[c:14]([cH:13][cH:12][cH:11]3)[NH:5][C:6](=O)[CH2:7][N:8]4[C@H:20]2[CH2:19][CH2:18]1>>[CH3:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][N:8]2[c:9]3[c:10]([cH:11][cH:12][cH:13][c:14]31)[C@@H:15]1[CH2:16][NH:17][CH2:18][CH2:19][C@H:20]21
CCCCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3
CCCCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
260fe71a473b60bc6699adc87a714c283b8e75d0d15e5c63eedaf0773c2c0554
5fa8b50dba8178d1bbd9e21cc84d8eae82649eda60ef87b4318bbafd818aae11
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CCN2
C-C-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4](-[C:5]-[C:6]-1)-[#7:7]1-[C:8]-[C;H0;D3;+0:9](=O)-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]-1.I-[CH2;D2;+0:14]-[C:15]-[C:16]>>[C:16]-[C:15]-[CH2;D2;+0:14]-[N;H0;D3;+0:10]1-[CH2;D2;+0:9]-[C:8]-[#7:7](-[c:13]:[c:11]-1:[c:12])-[C:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:6]-[C:5]-1
null
[]
null
null
null
null
Utilizing the material from Example 255 Step A, the title compound was prepared in analogous fashion using n-butyl iodide as the alkyl halide and following the procedure of Step B–D of Example 255, as a viscous brown liquid. 1H NMR (CDCl3, 300 Mhz) δ 0.95 (t, 3H), 1.30–1.45 (m, 2H), 1.50–1.65 (m, 2H), 1.95–2.15 (m, 2H)...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carbamic ester.Ether.Secondary amide
Secondary amine.Tertiary amine
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
HI
null
null
null
CCCCI.CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3>>CCCCN1CCN2c3c(cccc31)[C@@H]1CNCC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-613b4223845d4184ab9b9410adf77fb2
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.ICc1ccccc1>>c1ccc(CN2CCN3c4c(cccc42)[C@@H]2CNCC[C@@H]23)cc1
O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC.C(C1=CC=CC=C1)I>>C(C1=CC=CC=C1)N1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNC1
CCOC(=O)[N:18]1[CH2:17][C@H:16]2[c:11]3[c:10]4[c:15]([cH:14][cH:13][cH:12]3)[NH:6][C:7](=O)[CH2:8][N:9]4[C@H:21]2[CH2:20][CH2:19]1.I[CH2:5][c:4]1[cH:3][cH:2][cH:1][cH:23][cH:22]1>>[cH:1]1[cH:2][cH:3][c:4]([CH2:5][N:6]2[CH2:7][CH2:8][N:9]3[c:10]4[c:11]([cH:12][cH:13][cH:14][c:15]42)[C@@H:16]2[CH2:17][NH:18][CH2:19][CH2:...
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.ICc1ccccc1
c1ccc(CN2CCN3c4c(cccc42)[C@@H]2CNCC[C@@H]23)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
260fe71a473b60bc6699adc87a714c283b8e75d0d15e5c63eedaf0773c2c0554
5fa8b50dba8178d1bbd9e21cc84d8eae82649eda60ef87b4318bbafd818aae11
c1ccc(CN2CCN3c4c(cccc42)[C@@H]2CNCC[C@@H]23)cc1
C-C-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4](-[C:5]-[C:6]-1)-[#7:7]1-[C:8]-[C;H0;D3;+0:9](=O)-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]-1.I-[CH2;D2;+0:14]-[c:15](:[c:16]):[c:17]>>[c:12]:[c:11]1:[c:13]-[#7:7](-[C:8]-[CH2;D2;+0:9]-[N;H0;D3;+0:10]-1-[CH2;D2;+0:14]-[c:15](:[c:16]):[c:17])-[C:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:6]-...
null
[]
null
null
null
null
Utilizing the material from Example 255 Step A, the title compound was prepared in analogous fashion using benzyl iodide as the alkyl halide and following the procedure of Step B–D of Example 255, as a viscous liquid. 1H NMR(CDCl3, 300 MHz) δ 1.60–2.0 (m, 2H), 2.55–2.95(m, 4H), 2.95–3.15 (m, 2H), 3.20–3.45 (m, 3H), 4.4...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carbamic ester.Ether.Secondary amide
Secondary amine.Tertiary amine
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1ccccc1.c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
HI
null
null
null
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.ICc1ccccc1>>c1ccc(CN2CCN3c4c(cccc42)[C@@H]2CNCC[C@@H]23)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0b2e77a8efa445b4910a2f1651cba09e
CN1CCN2c3c(cccc31)[C@H]1CN(CCCC(=O)c3ccc(F)cc3)CC[C@H]12>>CN1CCN2c3c(cccc31)[C@@H]1CN(CCCC(=O)c3ccc(F)cc3)CC[C@@H]12
CN1CCN2C=3C(=CC=CC13)[C@@H]1[C@H]2CCN(C1)CCCC(=O)C1=CC=C(C=C1)F>>CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(C1)CCCC(=O)C1=CC=C(C=C1)F
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[C@H:12]1[CH2:13][N:14]([CH2:15][CH2:16][CH2:17][C:18](=[O:19])[c:20]3[cH:21][cH:22][c:23]([F:24])[cH:25][cH:26]3)[CH2:27][CH2:28][C@@H:29]21>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[C@@H:12]1[CH2:13][N:14]([CH2:1...
CN1CCN2c3c(cccc31)[C@H]1CN(CCCC(=O)c3ccc(F)cc3)CC[C@H]12
CN1CCN2c3c(cccc31)[C@@H]1CN(CCCC(=O)c3ccc(F)cc3)CC[C@@H]12
null
null
C(Cl)(Cl)Cl
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
O=C(CCCN1CC[C@H]2[C@@H](C1)c1cccc3c1N2CCN3)c1ccccc1
null
null
[]
null
null
null
null
The above compound was resolved into its enantiomers on chiral HPLC column. 4-((6bS,10aR)-3-methyl-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxalin-8(7H)-yl)-1-(4-fluorophenyl)-1-butanone. Viscous tan liquid. [a]D=−36.8° (c=0.886, CHCl3). MS (CI): 394 (M+H+). Conditions: See reaction.notes.proc...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
null
C(Cl)(Cl)Cl
null
null
CN1CCN2c3c(cccc31)[C@H]1CN(CCCC(=O)c3ccc(F)cc3)CC[C@H]12>C(Cl)(Cl)Cl>CN1CCN2c3c(cccc31)[C@@H]1CN(CCCC(=O)c3ccc(F)cc3)CC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-978cf607a84f46d4982b87aa73d09631
CN1C(=O)CN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12>>CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12
CC=1C=CC=CC1C.C=CCCCCCC.ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CC(N(C3C1)C)=O)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C.B.C1CCOC1>>ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCN(C3C1)C)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C
O=[C:3]1[N:2]([CH3:1])[c:19]2[c:6]3[c:7]([cH:8][c:9](-[c:10]4[cH:11][cH:12][c:13]([Cl:14])[cH:15][c:16]4[Cl:17])[cH:18]2)[C@@H:20]2[CH2:21][N:22]([C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29])[CH2:30][CH2:31][C@@H:32]2[N:5]3[CH2:4]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][c:9](-[c:10]4[cH:11][cH:...
CN1C(=O)CN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12
CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12
null
null
C1CCOC1
Reduction
Reduction of tertiary amides to amines
b85edbb5fb9a189d3d5456aab7a3bf994122238d91275bcbace6c7a052dc91bc
c8f3c617792f7a4fae96b8a97dc0ce23461ab85d8a738fe6caacff776ef51ffa
c1ccc(-c2cc3c4c(c2)[C@@H]2CNCC[C@@H]2N4CCN3)cc1
O=[C;H0;D3;+0:1]1-[C:2]-[#7:3](-[C:4])-[c:5]:[c:6]-[#7:7]-1-[C;D1;H3:8]>>[C:4]-[#7:3]1-[C:2]-[CH2;D2;+0:1]-[#7:7](-[C;D1;H3:8])-[c:6]:[c:5]-1
58
[{"value": 58.0, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCN(C3C1)C)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 50.2, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCN(C3C1)C)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false...
null
null
null
null
To a solution of tert-butyl (6bR,10aS)-5-(2,4-dichlorophenyl)-3-methyl-2-oxo-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (100 mg, 0.21 mmol) in THF (5.0 mL), BH3-THF (1M in THF) (0.82 mL, 0.82 mmol) was added dropwise. After addition was completed, the resulting reaction...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
null
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1ccccc1.c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
Other
C1CCOC1
null
null
CN1C(=O)CN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12>C1CCOC1>CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c9ff34fccf9a40a6b3e88db116cbc8cf
CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12>>CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CNCC[C@@H]12
ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCN(C3C1)C)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C.[OH-].[Na+]>>ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCN(C3C1)C)[C@@H]1[C@H]2CNCC1
CC(C)(C)OC(=O)[N:22]1[CH2:21][C@H:20]2[c:7]3[c:6]4[c:19]([cH:18][c:9](-[c:10]5[cH:11][cH:12][c:13]([Cl:14])[cH:15][c:16]5[Cl:17])[cH:8]3)[N:2]([CH3:1])[CH2:3][CH2:4][N:5]4[C@H:25]2[CH2:24][CH2:23]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][c:9](-[c:10]4[cH:11][cH:12][c:13]([Cl:14])[cH:15][c:16]4[Cl:17])[cH:1...
CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12
CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CNCC[C@@H]12
null
null
null
Reduction
Boc amine deprotection
c8e9e752815bb790c1e130bdaeff142903f3fdbe5557ab9e7c4e97add5d41c6b
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc(-c2cc3c4c(c2)[C@@H]2CNCC[C@@H]2N4CCN3)cc1
C-C(-C)(-C)-O-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]
80
[{"value": 80.0, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCN(C3C1)C)[C@@H]1[C@H]2CNCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.6, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCN(C3C1)C)[C@@H]1[C@H]2CNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The hydrochloride salt of the title compound was prepared from tert-butyl (6bR,10aS)-5-(2,4-dichlorophenyl)-3-methyl-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (50 mg) using the deprotection procedures described in Example 275, Step B. The salt formed was free-based wit...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
c1ccccc1.c1cc2c3c(c1)[C@@H]1CNCC[C@@H]1N3CC[NH]2
HO-
null
null
null
CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CN(C(=O)OC(C)(C)C)CC[C@@H]12>>CN1CCN2c3c(cc(-c4ccc(Cl)cc4Cl)cc31)[C@@H]1CNCC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7284b827a7f341c185594aec89c7eb91
CC(C)(C)OC(=O)N1CC[C@H]2[C@@H](C1)c1cc(Br)cc3c1N2CCN3.OB(O)c1ccc(Cl)cc1Cl>>CC(C)(C)OC(=O)N1CC[C@H]2[C@@H](C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CCN3
BrC=1C=C2C=3N(CCNC3C1)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C.ClC1=C(C=CC(=C1)Cl)B(O)O>>ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCNC3C1)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C
Br[c:16]1[cH:15][c:14]2[c:27]3[c:26]([cH:25]1)[NH:31][CH2:30][CH2:29][N:28]3[C@H:11]1[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:13][C@H:12]12.OB(O)[c:17]1[cH:18][cH:19][c:20]([Cl:21])[cH:22][c:23]1[Cl:24]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C@H:11]2[C@@...
CC(C)(C)OC(=O)N1CC[C@H]2[C@@H](C1)c1cc(Br)cc3c1N2CCN3.OB(O)c1ccc(Cl)cc1Cl
CC(C)(C)OC(=O)N1CC[C@H]2[C@@H](C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CCN3
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
7e0a80666e22e30220b2f360ec85e8bd8d76adda934c7385240ddcd629f581f2
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cc3c4c(c2)[C@@H]2CNCC[C@@H]2N4CCN3)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]-[#7:6].O-B(-O)-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:10](-[Cl;D1;H0:11]):[c:12]>>[#7:6]-[c:5]:[c:4]:[c;H0;D3;+0:1](-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:10](-[Cl;D1;H0:11]):[c:12]):[c:2]:[c:3]
61.8
[{"value": 60.0, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCNC3C1)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 61.8, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CCNC3C1)[C@@H]1[C@H]2CN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Tert-butyl (6bR,10aS)-5-(2,4-dichlorophenyl)-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (37 mg, 60%) was prepared via coupling of tert-butyl (6bR,10aS)-5-bromo-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (50 mg, 0.13 mmol...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2.c1ccccc1
c1ccccc1.c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1ccccc1.c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
HBr.B
null
null
null
CC(C)(C)OC(=O)N1CC[C@H]2[C@@H](C1)c1cc(Br)cc3c1N2CCN3.OB(O)c1ccc(Cl)cc1Cl>>CC(C)(C)OC(=O)N1CC[C@H]2[C@@H](C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CCN3
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-89bcdbe2e2ba44b9afe24a7112355d9b
CC(C)(C)OC(=O)N1CCc2[nH]c3c([N+](=O)[O-])cccc3c2C1>>CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1
[N+](=O)([O-])C1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C>>NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C
O=[N+:15]([O-])[c:14]1[c:13]2[nH:12][c:11]3[c:20]([c:19]2[cH:18][cH:17][cH:16]1)[CH2:21][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][CH2:10]3>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][c:11]2[nH:12][c:13]3[c:14]([NH2:15])[cH:16][cH:17][cH:18][c:19]3[c:20]2[CH2:21]1
CC(C)(C)OC(=O)N1CCc2[nH]c3c([N+](=O)[O-])cccc3c2C1
CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1
null
[Pd]
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2c3c([nH]c2c1)CCNC3
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]
null
[]
null
null
2
HOUR
To a solution of tert-butyl 6-nitro-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate (15.6 g, 49.15 mmol) in ethanol (250 mL) was added a spatula tip of 10% Pd/C. The reaction mixture was shaken under a hydrogen atmosphere (15 psi, Parr apparatus) for 2 h. Upon removal from the Parr apparatus, the reaction mixtu...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2c3c(nc2c1)CC[N]C3
Other
[Pd].C(C)O
null
2
CC(C)(C)OC(=O)N1CCc2[nH]c3c([N+](=O)[O-])cccc3c2C1>[Pd].C(C)O>CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-64eff7afe50445debf039097bbec1f7c
CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1.O=C(Cl)CCCl>>CC(C)(C)OC(=O)N1CCc2[nH]c3c(NC(=O)CCCl)cccc3c2C1
NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C.ClCCC(=O)Cl.C([O-])(O)=O.[Na+]>>ClCCC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][c:11]2[nH:12][c:13]3[c:14]([NH2:15])[cH:21][cH:22][cH:23][c:24]3[c:25]2[CH2:26]1.Cl[C:16](=[O:17])[CH2:18][CH2:19][Cl:20]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][c:11]2[nH:12][c:13]3[c:14]([NH:15][C:16](=[O:17])[CH2:18]...
CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1.O=C(Cl)CCCl
CC(C)(C)OC(=O)N1CCc2[nH]c3c(NC(=O)CCCl)cccc3c2C1
null
CN(C)C=1C=CN=CC1
C1=CC=CC=C1
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc2c3c([nH]c2c1)CCNC3
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8](:[c:9]):[#7;a:10]:[c:11]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8](:[c:9]):[#7;a:10]:[c:11]
99
[{"value": 99.0, "product": "ClCCC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
To a solution of tert-butyl 6-amino-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate (4.62 g, 16.08 mmol) in benzene (100 mL) was added a catalytic amount of DMAP. An inert atmosphere was created and chloropropionyl chloride (2)(1.68 mL) was added dropwise to the reaction mixture. After stirring at room temperat...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2c3c(nc2c1)CC[N]C3
HCl
CN(C)C=1C=CN=CC1.C1=CC=CC=C1
null
0.333333
CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1.O=C(Cl)CCCl>CN(C)C=1C=CN=CC1.C1=CC=CC=C1>CC(C)(C)OC(=O)N1CCc2[nH]c3c(NC(=O)CCCl)cccc3c2C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c2461e898ce941879538b46d3bf81bff
CN1CCN2c3c(cccc31)[C@@H]1CCN(C(=O)OC(C)(C)C)CC[C@@H]12>>CN1CCN2c3c(cccc31)[C@@H]1CCNCC[C@@H]12
CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCN(CC1)C(=O)OC(C)(C)C.[OH-].[Na+]>>CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNCC1
CC(C)(C)OC(=O)[N:15]1[CH2:14][CH2:13][C@H:12]2[c:7]3[c:6]4[c:11]([cH:10][cH:9][cH:8]3)[N:2]([CH3:1])[CH2:3][CH2:4][N:5]4[C@H:18]2[CH2:17][CH2:16]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[C@@H:12]1[CH2:13][CH2:14][NH:15][CH2:16][CH2:17][C@H:18]21
CN1CCN2c3c(cccc31)[C@@H]1CCN(C(=O)OC(C)(C)C)CC[C@@H]12
CN1CCN2c3c(cccc31)[C@@H]1CCNCC[C@@H]12
null
null
[Cl-].[Na+].O.C(Cl)Cl.C(=O)(C(F)(F)F)O
Reduction
Boc amine deprotection
6b2d5918b1bbb62a1da148ba095b4c22cda264c0445468ade141c385258ecbff
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc2c3c(c1)[C@@H]1CCNCC[C@@H]1N3CCN2
C-C(-C)(-C)-O-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]
104.7
[{"value": 103.0, "product": "CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 104.7, "product": "CN1CCN2C=3C(=CC=CC13)[C@H]1[C@@H]2CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2.5
HOUR
Tert-butyl (6bS,11aS)-3-methyl-2,3,6b,7,8,10,11,11a-octahydro-1H,9H-azepino[4′,5′:4,5]pyrrolo[1,2,3-de]quinoxaline-9-carboxylate (115 mg, 0.33 mmol) was dissolved in 20% TFA (3 mL) in CH2Cl2 at rt. The reaction was stirred at rt for 2.5 hrs. Ice chips were added to the reaction, an then it was basified with 50% NaOH un...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
c1cc2c3c(c1)[C@@H]1CC[NH]CC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CCNCC[C@@H]1N3CC[NH]2
c1cc2c3c(c1)[C@@H]1CCNCC[C@@H]1N3CC[NH]2
HO-
[Cl-].[Na+].O.C(Cl)Cl.C(=O)(C(F)(F)F)O
null
2.5
CN1CCN2c3c(cccc31)[C@@H]1CCN(C(=O)OC(C)(C)C)CC[C@@H]12>[Cl-].[Na+].O.C(Cl)Cl.C(=O)(C(F)(F)F)O>CN1CCN2c3c(cccc31)[C@@H]1CCNCC[C@@H]12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-052d77e5abfc477fb5ee178b23b92fe0
CN1CCN2c3c(cccc31)C1CCNCCC12.O=C(CCCCl)c1ccc(F)cc1>>CN1CCN2c3c(cccc31)C1CCN(CCCC(=O)c3ccc(F)cc3)CCC12
CN1CCN2C=3C(=CC=CC13)C1C2CCNCC1.ClCCCC(=O)C1=CC=C(C=C1)F.CCN(C(C)C)C(C)C>>CN1CCN2C=3C(=CC=CC13)C1C2CCN(CC1)CCCC(=O)C1=CC=C(C=C1)F
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[CH:12]1[CH2:13][CH2:14][NH:15][CH2:28][CH2:29][CH:30]21.Cl[CH2:16][CH2:17][CH2:18][C:19](=[O:20])[c:21]1[cH:22][cH:23][c:24]([F:25])[cH:26][cH:27]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]2[c:6]3[c:7]([cH:8][cH:9][cH:10][c:11]31)[CH:12]1[CH2:13][CH2:14]...
CN1CCN2c3c(cccc31)C1CCNCCC12.O=C(CCCCl)c1ccc(F)cc1
CN1CCN2c3c(cccc31)C1CCN(CCCC(=O)c3ccc(F)cc3)CCC12
null
null
O1CCOCC1
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
78309cea36c4b57c3488d59cbc25b7f0249d7382f00d475ecdfbc90c1ee4feca
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C(CCCN1CCC2c3cccc4c3N(CCN4)C2CC1)c1ccccc1
Cl-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]=[O;D1;H0:5].[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]=[O;D1;H0:5])-[C:9]-[C:10]
31
[{"value": 31.0, "product": "CN1CCN2C=3C(=CC=CC13)C1C2CCN(CC1)CCCC(=O)C1=CC=C(C=C1)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 30.7, "product": "CN1CCN2C=3C(=CC=CC13)C1C2CCN(CC1)CCCC(=O)C1=CC=C(C=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
96
CELSIUS
18
HOUR
3-Methyl-2,3,7,8,9,10,11,11a-octahydro-1H,6bH-azepino[4′,5′:4,5]pyrrolo[1,2,3-de]quinoxaline (72 mg, 0.3 mmol), 4-chloro-4′-flourobutyrophenone (119 mg, 0.6 mmol), KI (49 mg, 0.3 mmol), and DIEA (383 mg, 3 mmol) were added to dioxane (2.5 mL). The suspension was stirred at 96° C. for 18 hrs. The reaction was cooled to ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
c1cc2c3c(c1)C1CCNCCC1N3CC[NH]2
c1cc2c3c(c1)C1CC[NH]CCC1N3CC[NH]2
c1ccccc1.c1cc2c3c(c1)C1CC[NH]CCC1N3CC[NH]2
HCl
O1CCOCC1
96
18
CN1CCN2c3c(cccc31)C1CCNCCC12.O=C(CCCCl)c1ccc(F)cc1>O1CCOCC1>CN1CCN2c3c(cccc31)C1CCN(CCCC(=O)c3ccc(F)cc3)CCC12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cf8e8b15a9a04ebea52f5a2bf85cca00
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI>>CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)C(=O)N4C)C1
O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC.[H-].[Na+].CI.CN(C)C=O>>CC1(C(N(C=2C=CC=C3C2N1C1=C3CN(CC1)C(=O)OCC)C)=O)C
[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][C@H:9]2[C@H:10]([c:11]3[cH:12][cH:13][cH:14][c:15]4[c:16]3[N:17]2[CH2:18][C:21](=[O:22])[NH:23]4)[CH2:25]1.I[CH3:24]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][c:9]2[c:10]([c:11]3[cH:12][cH:13][cH:14][c:15]4[c:16]3[n:17]2[C:18]([CH3:19])([CH3:20])[C:21](=[...
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)C(=O)N4C)C1
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
752a8786c40f1841769d3c150929e814462d11724e0dd540f9edf1f45e586905
8c44445309ae5ab70d1a3b7f1a9d955e701b46095afe5c0bf4042a19b519dbd1
O=C1Cn2c3c(c4cccc(c42)N1)CNCC3
I-[CH3;D1;+0:1].[#8:2]-[C:3](=[O;D1;H0:4])-[#7:5]1-[C:6]-[C@@H;D3;+0:7]2-[C@H;D3;+0:8](-[C:9]-[C:10]-1)-[N;H0;D3;+0:11]1-[CH2;D2;+0:12]-[C:13](=[O;D1;H0:14])-[NH;D2;+0:15]-[c:16](:[c:17]):[c:18]-1:[c:19]-2:[c:20]>>[#8:2]-[C:3](=[O;D1;H0:4])-[#7:5]1-[C:6]-[c;H0;D3;+0:7]2:[c:19](:[c:20]):[c:18]3:[c:16](:[c:17])-[N;H0;D3;...
90
[{"value": 90.0, "product": "CC1(C(N(C=2C=CC=C3C2N1C1=C3CN(CC1)C(=O)OCC)C)=O)C", "details": "PERCENTYIELD", "is_desired": false}]
25
CELSIUS
6
HOUR
To a solution of ethyl 2-oxo-2,3,9,10-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (from Example 211, Step A) (360 mg, 1.2 mmol) in DMF (20 mL) at rt was added NaH (172 mg, 4.8 mmol), MeI (0.25 mL, 4.0 mmol) and stirred at 25° C. for 6 hours. The solution was diluted with water (30 mL) ...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Tertiary amine
Tertiary amide
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)c1c(n3CC[NH]2)CC[NH]C1
c1cc2c3c(c1)c1c(n3CC[NH]2)CC[NH]C1
I-
O
25
6
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI>O>CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)C(=O)N4C)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2e890b6654fc4022af6146dc53482ebb
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)C(=O)N4C)C1>>CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)CN4C)C1
CC1(C(N(C=2C=CC=C3C2N1C1=C3CN(CC1)C(=O)OCC)C)=O)C.Cl.O>>C(C)OC(=O)N1CC2=C(N3C(CN(C=4C=CC=C2C34)C)(C)C)CC1
O=[C:21]1[C:18]([CH3:19])([CH3:20])[n:17]2[c:9]3[c:10]([c:11]4[cH:12][cH:13][cH:14][c:15]([c:16]42)[N:22]1[CH3:23])[CH2:24][N:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][CH2:8]3>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][c:9]2[c:10]([c:11]3[cH:12][cH:13][cH:14][c:15]4[c:16]3[n:17]2[C:18]([CH3:19])([CH3:20])[...
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)C(=O)N4C)C1
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)CN4C)C1
null
null
C1CCOC1
Reduction
Reduction of tertiary amides to amines
5fa3a89ad4a5f755ae33c982f253a7fc08686eefa0997651ea69b1e0b6f3df23
c8f3c617792f7a4fae96b8a97dc0ce23461ab85d8a738fe6caacff776ef51ffa
c1cc2c3c(c1)c1c(n3CCN2)CCNC1
O=[C;H0;D3;+0:1]1-[#7:2](-[C;D1;H3:3])-[c:4]:[c:5]:[#7;a:6](:[c:7])-[C:8]-1(-[C;D1;H3:9])-[C;D1;H3:10]>>[C;D1;H3:9]-[C:8]1(-[C;D1;H3:10])-[CH2;D2;+0:1]-[#7:2](-[C;D1;H3:3])-[c:4]:[c:5]:[#7;a:6]-1:[c:7]
66.3
[{"value": 66.0, "product": "C(C)OC(=O)N1CC2=C(N3C(CN(C=4C=CC=C2C34)C)(C)C)CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 66.3, "product": "C(C)OC(=O)N1CC2=C(N3C(CN(C=4C=CC=C2C34)C)(C)C)CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
5
HOUR
To a solution of ethyl 1,1,3-trimethyl-2-oxo-2,3,9,10-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (240 mg, 0.7 mmol) in THF (20 mL) at 25° C. was added BH3/THF complex (0.7 mL, 0.7 mmol). The mixture was stirred at 80° C. for 5 hours then cooled to rt and added 6N HCl (10 mL) with stir...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
null
c1cc2c3c(c1)c1c(n3CC[NH]2)CC[NH]C1
c1cc2c3c(c1)c1c(n3CC[NH]2)CC[NH]C1
c1cc2c3c(c1)c1c(n3CC[NH]2)CC[NH]C1
Other
C1CCOC1
80
5
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)C(=O)N4C)C1>C1CCOC1>CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)CN4C)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-839480f60904490981a35ec588a9f443
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)CN4C)C1>>CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(C)(C)CN3C
C(C)OC(=O)N1CC2=C(N3C(CN(C=4C=CC=C2C34)C)(C)C)CC1.[BH3-]C#N.[Na+]>>C(C)OC(=O)N1CC2C(N3C(CN(C=4C=CC=C2C34)C)(C)C)CC1
[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][c:9]2[c:10]([c:12]3[cH:13][cH:14][cH:15][c:16]4[c:17]3[n:18]2[C:19]([CH3:20])([CH3:21])[CH2:22][N:23]4[CH3:24])[CH2:11]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH:9]2[CH:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:17]1[N:18]2[C:19]([CH3:20])([C...
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)CN4C)C1
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(C)(C)CN3C
null
null
C(=O)(C(F)(F)F)O
Reduction
OtherReaction
340cf53908efa49cc662c219bf9df412f1d128f5373473fd3c1f2437e4111407
3f9bd1254c561719832bd71149feb4e99c5764db1feb47bf9fbdfb1c414d602b
c1cc2c3c(c1)C1CNCCC1N3CCN2
[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[c;H0;D3;+0:6]2:[c:7](:[c:8]):[c:9]3:[c:10]-[#7:11]-[C:12]-[C:13](-[C;D1;H3:14])(-[C;D1;H3:15])-[n;H0;D3;+0:16]:3:[c;H0;D3;+0:17]:2-[C:18]-[C:19]-1>>[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[CH;D3;+0:6]2-[CH;D3;+0:17](-[C:18]-[C:19]-1)-[N;H0;D3;+0:16]1-[c:9](:[c:10]-[#7:11]-[C:1...
null
[]
null
null
4
HOUR
To a solution of ethyl-1,1,3-trimethyl-2,3,9,10-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (69 mg, 0.21 mmol) in TFA (2 mL) at 0° C. was added NaBH3CN (53 mg, 0.84 mmol). The mixture was stirred at rt for 4 hours, and then removed the TFA by N2. About 10 mL of H2O was added and then w...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amine
c1cc2c3c(c1)c1c(n3CC[NH]2)CC[NH]C1
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
null
C(=O)(C(F)(F)F)O
null
4
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)(C)CN4C)C1>C(=O)(C(F)(F)F)O>CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(C)(C)CN3C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c32e62ca360e4113b29284295ba445c8
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(C)(C)CN3C>>CN1CC(C)(C)N2c3c(cccc31)C1CNCCC12
CC1(CN(C=2C=CC=C3C2N1C1C3CN(CC1)C(=O)OCC)C)C.[OH-].[K+]>>CC1(CN(C=2C=CC=C3C2N1C1C3CNCC1)C)C
CCOC(=O)[N:16]1[CH2:15][CH:14]2[c:9]3[c:8]4[c:13]([cH:12][cH:11][cH:10]3)[N:2]([CH3:1])[CH2:3][C:4]([CH3:5])([CH3:6])[N:7]4[CH:19]2[CH2:18][CH2:17]1>>[CH3:1][N:2]1[CH2:3][C:4]([CH3:5])([CH3:6])[N:7]2[c:8]3[c:9]([cH:10][cH:11][cH:12][c:13]31)[CH:14]1[CH2:15][NH:16][CH2:17][CH2:18][CH:19]21
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(C)(C)CN3C
CN1CC(C)(C)N2c3c(cccc31)C1CNCCC12
null
null
O.C(CCC)O
Reduction
Hydrogenolysis of tertiary amines
f02ea03182ae60dba06bafd552caf7571f18d68abb977b141f1d2eed23563f1d
20c36f41eeb07c3ba4437b51ba72e8ff3c22d0b27e7197b0e9af3127f331149f
c1cc2c3c(c1)C1CNCCC1N3CCN2
C-C-O-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]
97.1
[{"value": 81.0, "product": "CC1(CN(C=2C=CC=C3C2N1C1C3CNCC1)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.1, "product": "CC1(CN(C=2C=CC=C3C2N1C1C3CNCC1)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
120
CELSIUS
20
HOUR
To a solution of ethyl 1,1,3-trimethyl-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (8 mg, 0.02 mmol) in n-butanol (5 mL) at rt was added KOH (50 mg, 0.89 mmol) and stirred at 120° C. for 20 hours. The solution was diluted with water (10 mL) and extracted with EtOAc (2×20...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether
Secondary amine
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1CNCCC1N3CC[NH]2
c1cc2c3c(c1)C1CNCCC1N3CC[NH]2
HO-
O.C(CCC)O
120
20
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(C)(C)CN3C>O.C(CCC)O>CN1CC(C)(C)N2c3c(cccc31)C1CNCCC12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-38abd261a10a4ad5a41e06e9071cc622
CN1CC(C)(C)N2c3c(cccc31)C1CNCCC12.O=C(CCCCl)c1ccc(F)cc1>>CN1CC(C)(C)N2c3c(cccc31)C1CN(CCCC(=O)c3ccc(F)cc3)CCC12
CC1(CN(C=2C=CC=C3C2N1C1C3CNCC1)C)C.ClCCCC(=O)C1=CC=C(C=C1)F.C(=O)([O-])[O-].[K+].[K+]>>FC1=CC=C(C=C1)C(CCCN1CC2C(N3C(CN(C=4C=CC=C2C34)C)(C)C)CC1)=O
[CH3:1][N:2]1[CH2:3][C:4]([CH3:5])([CH3:6])[N:7]2[c:8]3[c:9]([cH:10][cH:11][cH:12][c:13]31)[CH:14]1[CH2:15][NH:16][CH2:29][CH2:30][CH:31]21.Cl[CH2:17][CH2:18][CH2:19][C:20](=[O:21])[c:22]1[cH:23][cH:24][c:25]([F:26])[cH:27][cH:28]1>>[CH3:1][N:2]1[CH2:3][C:4]([CH3:5])([CH3:6])[N:7]2[c:8]3[c:9]([cH:10][cH:11][cH:12][c:13...
CN1CC(C)(C)N2c3c(cccc31)C1CNCCC12.O=C(CCCCl)c1ccc(F)cc1
CN1CC(C)(C)N2c3c(cccc31)C1CN(CCCC(=O)c3ccc(F)cc3)CCC12
null
null
O1CCOCC1.O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
54f03545a14958e98f0e3ee8166420a409e56e78b56c8c4176a28619af3af9b3
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C(CCCN1CCC2C(C1)c1cccc3c1N2CCN3)c1ccccc1
Cl-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]=[O;D1;H0:5].[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]=[O;D1;H0:5])-[C:9]-[C:10]
43
[{"value": 43.0, "product": "FC1=CC=C(C=C1)C(CCCN1CC2C(N3C(CN(C=4C=CC=C2C34)C)(C)C)CC1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 43.0, "product": "FC1=CC=C(C=C1)C(CCCN1CC2C(N3C(CN(C=4C=CC=C2C34)C)(C)C)CC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
25
CELSIUS
24
HOUR
To a solution of 1,1,3-trimethyl-2,3,6b,7,8,9,10,10a-octahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline (from Example 283) (82 mg, 0.32 mmol) in dioxane (10 mL) at rt was added 4-chloro-1-(4-fluorophenyl)butan-1-one (83 mg, 0.42 mmol), K2CO3 (100 mg), KI (30 mg) and stirred at 25° C. for 24 hours. The solution ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
c1cc2c3c(c1)C1CNCCC1N3CC[NH]2
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1ccccc1.c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
HCl
O1CCOCC1.O
25
24
CN1CC(C)(C)N2c3c(cccc31)C1CNCCC12.O=C(CCCCl)c1ccc(F)cc1>O1CCOCC1.O>CN1CC(C)(C)N2c3c(cccc31)C1CN(CCCC(=O)c3ccc(F)cc3)CCC12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b9ca7c7471ad47b7a02b8cc327b4d882
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI.CN(C)C=O>>CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)C(=O)N4C)C1
O=C1NC=2C=CC=C3C2N(C1)[C@@H]1[C@H]3CN(CC1)C(=O)OCC.[H-].[Na+].CI.CN(C)C=O>>CC1C(N(C=2C=CC=C3C2N1C1=C3CN(CC1)C(=O)OCC)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][C@H:9]2[C@H:10]([c:11]3[cH:12][cH:13][cH:14][c:15]4[c:16]3[N:17]2[CH2:18][C:20](=[O:21])[NH:22]4)[CH2:24]1.I[CH3:19].CN(C=O)[CH3:23]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][c:9]2[c:10]([c:11]3[cH:12][cH:13][cH:14][c:15]4[c:16]3[n:17]2[CH:18]([CH3:19])[C...
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI.CN(C)C=O
CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)C(=O)N4C)C1
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
075d82b4553c6e43466d8f93081af660d16d95e41691a0a0b207cf8665b828b7
6e2a0303410aaf9252fae4e16a65d95bbe41a60005164311b105893830bea4a6
O=C1Cn2c3c(c4cccc(c42)N1)CNCC3
C-N(-[CH3;D1;+0:1])-C=O.I-[CH3;D1;+0:2].[#8:3]-[C:4](=[O;D1;H0:5])-[#7:6]1-[C:7]-[C@@H;D3;+0:8]2-[C@H;D3;+0:9](-[C:10]-[C:11]-1)-[N;H0;D3;+0:12]1-[CH2;D2;+0:13]-[C:14](=[O;D1;H0:15])-[NH;D2;+0:16]-[c:17](:[c:18]):[c:19]-1:[c:20]-2:[c:21]>>[#8:3]-[C:4](=[O;D1;H0:5])-[#7:6]1-[C:7]-[c;H0;D3;+0:8]2:[c:20](:[c:21]):[c:19]3:...
64
[{"value": 64.0, "product": "CC1C(N(C=2C=CC=C3C2N1C1=C3CN(CC1)C(=O)OCC)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
25
CELSIUS
3
HOUR
To a solution of ethyl 2-oxo-2,3,9,10-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (from Example 211, Step A) (500 mg, 1.6 mmol) in DMF (20 mL) at rt was added NaH (147 mg, 3.6 mmol), MeI (0.25 mL, 4.0 mmol) and stirred at 25° C. for 3 hours. The solution was diluted with water (30 mL) ...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Tertiary amide.Tertiary amine
Tertiary amide
c1cc2c3c(c1)[C@@H]1C[NH]CC[C@@H]1N3CCN2
c1cc2c3c(c1)c1c(n3CC[NH]2)CC[NH]C1
c1cc2c3c(c1)c1c(n3CC[NH]2)CC[NH]C1
HI
O
25
3
CCOC(=O)N1CC[C@H]2[C@@H](C1)c1cccc3c1N2CC(=O)N3.CI.CN(C)C=O>O>CCOC(=O)N1CCc2c(c3cccc4c3n2C(C)C(=O)N4C)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-da2acf2b79e44ac089ddfca403fc215e
CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1.CCOC(=O)Cl>>CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OC(C)(C)C)C3
NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C.C(=O)([O-])[O-].[K+].[K+].ClC(=O)OCC>>C(C)OC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C
[NH2:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]3[c:13]([nH:14][c:15]12)[CH2:16][CH2:17][N:18]([C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])[CH2:26]3.Cl[C:4]([O:3][CH2:2][CH3:1])=[O:5]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]3[c:13]([nH:14][c:15]12)[CH2:16][CH2:17][N:18]([C:...
CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1.CCOC(=O)Cl
CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OC(C)(C)C)C3
null
null
O.C(Cl)Cl
Protection
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
038720aa61a7efa0f2a9ee6f2e0adf63a9ffdc2be4697c11a6215baef34f97b2
205f353513ce9506ab61831799da8fb73ec2ef5cfa927664496d3ce72c438860
c1ccc2c3c([nH]c2c1)CCNC3
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8](:[c:9]):[#7;a:10]:[c:11]>>[C:4]-[#8:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8](:[c:9]):[#7;a:10]:[c:11]
605.1
[{"value": 100.0, "product": "C(C)OC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 605.1, "product": "C(C)OC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
25
CELSIUS
0.5
HOUR
To a solution of tert-butyl 6-amino-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate (7 g, 24.3 mmol) in CH2Cl2 (40 mL) at rt was added saturated K2CO3 (30 mL), ethyl chloroformate (2.4 mL, 4.0 mmol) and stirred at 25° C. for 0.5 hour. The solution was diluted with water (30 mL) and extracted with CH2Cl2 (2×30 m...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether.Primary amine
Carbamic ester
null
null
c1ccc2c3c([nH]c2c1)CC[NH]C3
HCl
O.C(Cl)Cl
25
0.5
CC(C)(C)OC(=O)N1CCc2[nH]c3c(N)cccc3c2C1.CCOC(=O)Cl>O.C(Cl)Cl>CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OC(C)(C)C)C3
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5401a6a99e0e4a08b9bdab2e0357f4c7
CCOC(=O)Cl.CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OC(C)(C)C)C3>>CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OCC)C3
ClC(=O)OCC.C(=O)([O-])[O-].[K+].[K+].C(C)OC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OC(C)(C)C.C(=O)(C(F)(F)F)O>>C(C)OC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OCC
Cl[C:19](=[O:20])[O:21][CH2:22][CH3:23].CC(C)(C)OC(=O)[N:18]1[CH2:17][CH2:16][c:13]2[c:12]([c:11]3[cH:10][cH:9][cH:8][c:7]([NH:6][C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:15]3[nH:14]2)[CH2:24]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]3[c:13]([nH:14][c:15]12)[CH2:16][CH2:17][N:18]([C:19](=...
CCOC(=O)Cl.CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OC(C)(C)C)C3
CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OCC)C3
null
null
O.C(Cl)Cl
Protection
OtherReaction
0b45546f23ba96b2930821b82e0dc65795a0b0f131fefb23e532431874dc4e69
1a97805f72f7ff675aa3cc1da2d0cb1ed8f477704da937465d3c1e9310f62c42
c1ccc2c3c([nH]c2c1)CCNC3
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[c:4](:[#7;a:5]):[c:6]-[C:7]-1.Cl-[C;H0;D3;+0:8](=[O;D1;H0:9])-[#8:10]-[C:11]>>[#7;a:5]:[c:4]1:[c:6]-[C:7]-[N;H0;D3;+0:1](-[C;H0;D3;+0:8](=[O;D1;H0:9])-[#8:10]-[C:11])-[C:2]-[C:3]-1
67
[{"value": 67.0, "product": "C(C)OC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 55.9, "product": "C(C)OC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a solution of tert-butyl 6-[(ethoxycarbonyl)amino]-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate (8.7 g, 24.3 mmol) in CH2Cl2 (40 mL) at rt was added TFA (20 mL) and stirred at rt for 3 hours before the solvent was removed by the nitrogen stream. The solution was diluted with water (30 mL) and extracted wi...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Carbamic ester.Ether.Ether.Boc
Carbamic ester
c1ccc2c3c(nc2c1)CC[N]C3
c1ccc2c3c([nH]c2c1)CC[NH]C3
c1ccc2c3c([nH]c2c1)CC[NH]C3
HCl
O.C(Cl)Cl
null
3
CCOC(=O)Cl.CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OC(C)(C)C)C3>O.C(Cl)Cl>CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OCC)C3
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b5dd63660d0e4d47aea531cdc0d821dc
CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OCC)C3>>CCOC(=O)Nc1cccc2c1NC1CCN(C(=O)OCC)CC21
[BH3-]C#N.[Na+].C(C)OC(=O)NC1=CC=CC=2C3=C(NC12)CCN(C3)C(=O)OCC.C(=O)(C(F)(F)F)O>>C(C)OC(=O)NC1=CC=CC=2C3C(NC12)CCN(C3)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]1[nH:13][c:14]1[c:24]2[CH2:23][N:17]([C:18](=[O:19])[O:20][CH2:21][CH3:22])[CH2:16][CH2:15]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]1[NH:13][CH:14]1[CH2:15][CH2:16][N:17]([C:18](=[O:19])[O:20][CH2:21][CH3:2...
CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OCC)C3
CCOC(=O)Nc1cccc2c1NC1CCN(C(=O)OCC)CC21
null
null
C(Cl)Cl
Reduction
OtherReaction
07e512b90926111428bf112878dcfee6a9f535bae28cf741b34bf997102c8ce2
2b7f370a519e29b4dede190aa36b37f30822496e32f2c8bfa9736e631bde52e2
c1ccc2c(c1)NC1CCNCC21
[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[C:6]-[c;H0;D3;+0:7]2:[nH;D2;+0:8]:[c:9](:[c:10]):[c:11](:[c:12]):[c;H0;D3;+0:13]:2-[C:14]-1>>[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[C:6]-[CH;D3;+0:7]2-[NH;D2;+0:8]-[c:9](:[c:10]):[c:11](:[c:12])-[CH;D3;+0:13]-2-[C:14]-1
80
[{"value": 80.0, "product": "C(C)OC(=O)NC1=CC=CC=2C3C(NC12)CCN(C3)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.4, "product": "C(C)OC(=O)NC1=CC=CC=2C3C(NC12)CCN(C3)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a solution of ethyl 6-[(ethoxycarbonyl)amino]-1,3,4,5-tetrahydro-2H-pyrido[4,3-b]indole-2-carboxylate (4.5 g, 13.6 mmol) in CH2Cl2 (40 mL) at 0° C. was added TFA (20 mL) followed by NaCNBH3 (1.8 g, 27 mmol) and stirred at rt for 3 hours before the solvent was removed by the nitrogen stream. To the resulting residue ...
10.6084/m9.figshare.5104873.v1
null
null
Secondary amine
c1ccc2c3c([nH]c2c1)CC[NH]C3
c1ccc2c(c1)NC1CC[NH]CC21
c1ccc2c(c1)NC1CC[NH]CC21
null
C(Cl)Cl
null
3
CCOC(=O)Nc1cccc2c3c([nH]c12)CCN(C(=O)OCC)C3>C(Cl)Cl>CCOC(=O)Nc1cccc2c1NC1CCN(C(=O)OCC)CC21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-965cab1df3be4aa384b2495fed28e350
CC(=O)Cl.CCOC(=O)Nc1cccc2c1NC1CCN(C(=O)OCC)CC21>>CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)CN3C(=O)OCC
C(C)OC(=O)NC1=CC=CC=2C3C(NC12)CCN(C3)C(=O)OCC.[H-].[Na+].C(C)(=O)Cl>>O=C1CN(C=2C=CC=C3C2N1C1C3CN(CC1)C(=O)OCC)C(=O)OCC
Cl[C:19](=[O:20])[CH3:21].[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH:9]2[CH:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]([NH:22][C:23](=[O:24])[O:25][CH2:26][CH3:27])[c:17]1[NH:18]2>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH:9]2[CH:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:17]1[...
CC(=O)Cl.CCOC(=O)Nc1cccc2c1NC1CCN(C(=O)OCC)CC21
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)CN3C(=O)OCC
null
CN(C)C=1C=CN=CC1
O.CN(C)C=O
Protection
OtherReaction
32014f139d819d2eb766744258916273133b72bd014f22f00008a52addcf3b2a
1f98e4cf360ae4d501c8d71883b10df7f5adca46d6ffb377b7d7efe4e9374988
O=C1CNc2cccc3c2N1C1CCNCC31
Cl-[C;H0;D3;+0:1](-[CH3;D1;+0:2])=[O;D1;H0:3].[C:4]-[#8:5]-[C:6](=[O;D1;H0:7])-[NH;D2;+0:8]-[c:9](:[c:10]):[c:11]1:[c:12]-[C:13]-[C:14](-[C:15])-[NH;D2;+0:16]-1>>[C:4]-[#8:5]-[C:6](=[O;D1;H0:7])-[N;H0;D3;+0:8]1-[CH2;D2;+0:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[N;H0;D3;+0:16]2-[C:14](-[C:15])-[C:13]-[c:12]:[c:11]-2:[c:9]-1:[c...
57
[{"value": 57.0, "product": "O=C1CN(C=2C=CC=C3C2N1C1C3CN(CC1)C(=O)OCC)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 44.6, "product": "O=C1CN(C=2C=CC=C3C2N1C1C3CN(CC1)C(=O)OCC)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a solution of ethyl 6-[(ethoxycarbonyl)amino]-1,3,4,4a,5,9b-hexahydro-2H-pyrido[4,3-b]indole-2-carboxylate (2.2 g, 6.6 mmol) in DMF (20 mL) at 0° C. was added NaH (660 mg, 16.5 mmol), DMAP (878 mg, 7.2 mmol), acetyl chloride (0.6 mL, 7.2 mmol) and stirred at rt for 16 hours. The solution was diluted with water (30 m...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Carbamic ester.Secondary amine
Carbamic ester.Tertiary amide
c1ccc2c(c1)NC1CC[NH]CC21
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
HCl
CN(C)C=1C=CN=CC1.O.CN(C)C=O
null
16
CC(=O)Cl.CCOC(=O)Nc1cccc2c1NC1CCN(C(=O)OCC)CC21>CN(C)C=1C=CN=CC1.O.CN(C)C=O>CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)CN3C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1a37fbcebbb44045bf6f587865e2f566
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)CN3C(=O)OCC.CI>>CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)C(C)N3C(=O)OCC
O=C1CN(C=2C=CC=C3C2N1C1C3CN(CC1)C(=O)OCC)C(=O)OCC.[H-].[Na+].CI>>CC1N(C=2C=CC=C3C2N(C1=O)C1C3CN(CC1)C(=O)OCC)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH:9]2[CH:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:17]1[N:18]2[C:19](=[O:20])[CH2:21][N:23]3[C:24](=[O:25])[O:26][CH2:27][CH3:28].I[CH3:22]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH:9]2[CH:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:...
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)CN3C(=O)OCC.CI
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)C(C)N3C(=O)OCC
null
null
O.CN(C)C=O
C-C Coupling
Methylation with MeI_secondary
4e21c68c501a921c07db7be1b7940189d2eecde770dc3a568d774b11bef01893
410ec9b1cc243569e4ff568c248f0b402403802e002b4018f576af3f6960507b
O=C1CNc2cccc3c2N1C1CCNCC31
I-[CH3;D1;+0:1].[#8:2]-[C:3](=[O;D1;H0:4])-[#7:5]1-[CH2;D2;+0:6]-[C:7](=[O;D1;H0:8])-[#7:9](-[C:10])-[c:11]:[c:12]-1>>[#8:2]-[C:3](=[O;D1;H0:4])-[#7:5]1-[c:12]:[c:11]-[#7:9](-[C:10])-[C:7](=[O;D1;H0:8])-[CH;D3;+0:6]-1-[CH3;D1;+0:1]
80
[{"value": 80.0, "product": "CC1N(C=2C=CC=C3C2N(C1=O)C1C3CN(CC1)C(=O)OCC)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.8, "product": "CC1N(C=2C=CC=C3C2N(C1=O)C1C3CN(CC1)C(=O)OCC)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a solution of diethyl 1-oxo-6b,9,10,10a-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-3,8(2H,7H)-dicarboxylate (360 mg, 0.97 mmol) in DMF (20 mL) at 0° C. was added NaH (193 mg, 4.8 mmol), MeI (0.3 mL, 4.8 mmol) and stirred at rt for 16 hours. The solution was diluted with water (20 mL), and extracted ...
10.6084/m9.figshare.5104873.v1
null
null
null
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
HI
O.CN(C)C=O
null
16
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)CN3C(=O)OCC.CI>O.CN(C)C=O>CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)C(C)N3C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0d644445c2c049578ec7a710b1f2c5a7
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)C(C)N3C(=O)OCC>>CCOC(=O)N1CCC2C(C1)c1cccc3c1N2CC(C)N3C(=O)OCC
CC1N(C=2C=CC=C3C2N(C1=O)C1C3CN(CC1)C(=O)OCC)C(=O)OCC.Cl>>CC1N(C=2C=CC=C3C2N(C1)C1C3CN(CC1)C(=O)OCC)C(=O)OCC
O=[C:19]1[N:18]2[CH:9]3[CH2:8][CH2:7][N:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:11][CH:10]3[c:12]3[cH:13][cH:14][cH:15][c:16]([c:17]32)[N:22]([C:23](=[O:24])[O:25][CH2:26][CH3:27])[CH:20]1[CH3:21]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH:9]2[CH:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:15][c:16]3[c:17]1[N...
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)C(C)N3C(=O)OCC
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2CC(C)N3C(=O)OCC
null
null
O.C1CCOC1
Reduction
Reduction of tertiary amides to amines
f4b8adbbe1e8fda9e37d7419b5527bf584a957a3d24228e3b56a3b55bc1052ba
c8f3c617792f7a4fae96b8a97dc0ce23461ab85d8a738fe6caacff776ef51ffa
c1cc2c3c(c1)C1CNCCC1N3CCN2
O=[C;H0;D3;+0:1]1-[#7:2](-[C:3])-[c:4]:[c:5]-[#7:6](-[C:7](-[#8:8])=[O;D1;H0:9])-[C:10]-1-[C;D1;H3:11]>>[#8:8]-[C:7](=[O;D1;H0:9])-[#7:6]1-[c:5]:[c:4]-[#7:2](-[C:3])-[CH2;D2;+0:1]-[C:10]-1-[C;D1;H3:11]
69.6
[{"value": 69.0, "product": "CC1N(C=2C=CC=C3C2N(C1)C1C3CN(CC1)C(=O)OCC)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 69.6, "product": "CC1N(C=2C=CC=C3C2N(C1)C1C3CN(CC1)C(=O)OCC)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
To a solution of diethyl 2-methyl-1-oxo-6b,9,10,10a-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-3,8(2H,7H)-dicarboxylate (300 mg, 0.77 mmol) in THF (10 mL) at rt was added BH3THF complex (3.8 mL, 3.8 mmol) and refluxed for 5 hours. At rt 6N HCl (10 mL) was added and stirred for 0.5 hour before the solut...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
null
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
Other
O.C1CCOC1
null
0.5
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2C(=O)C(C)N3C(=O)OCC>O.C1CCOC1>CCOC(=O)N1CCC2C(C1)c1cccc3c1N2CC(C)N3C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5f7d81cfb0094974a5fcbeb091b6b912
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2CC(C)N3C(=O)OCC.O=C1CCC(=O)N1Br>>CCOC(=O)N1CCC2C(C1)c1cc(Br)cc3c1N2CC(C)N3C(=O)OCC
CC1N(C=2C=CC=C3C2N(C1)C1C3CN(CC1)C(=O)OCC)C(=O)OCC.C1CC(=O)N(C1=O)Br>>BrC=1C=C2C=3N(CC(N(C3C1)C(=O)OCC)C)C1C2CN(CC1)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH:9]2[CH:10]([CH2:11]1)[c:12]1[cH:13][cH:14][cH:16][c:17]3[c:18]1[N:19]2[CH2:20][CH:21]([CH3:22])[N:23]3[C:24](=[O:25])[O:26][CH2:27][CH3:28].O=C1CCC(=O)N1[Br:15]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH:9]2[CH:10]([CH2:11]1)[c:12]1[cH:13][c:14]([Br:...
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2CC(C)N3C(=O)OCC.O=C1CCC(=O)N1Br
CCOC(=O)N1CCC2C(C1)c1cc(Br)cc3c1N2CC(C)N3C(=O)OCC
null
null
O.CN(C)C=O
Functional Group Interconversion
Bromination
d2c26aee9f9ca727bf352a2d7b56fa077e1ffc4c2dc8ec5b01124d6118571879
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1cc2c3c(c1)C1CNCCC1N3CCN2
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[#7:2]-[c:3]:[c:4]:[cH;D2;+0:5]:[c:6]:[c:7]>>[#7:2]-[c:3]:[c:4]:[c;H0;D3;+0:5](-[Br;H0;D1;+0:1]):[c:6]:[c:7]
88.4
[{"value": 88.0, "product": "BrC=1C=C2C=3N(CC(N(C3C1)C(=O)OCC)C)C1C2CN(CC1)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 88.4, "product": "BrC=1C=C2C=3N(CC(N(C3C1)C(=O)OCC)C)C1C2CN(CC1)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
To a solution of diethyl 2-methyl-6b,9,10,10a-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-3,8(2H,7H)-dicarboxylate (40 mg, 0.1 mmol) in DMF (10 mL) at 0° C. was added NBS (20 mg, 0.11 mmol) and stirred at 0° C. for 2 hours. The solution was diluted with water (10 mL), and extracted with EtOAc (2×20 mL)....
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2.C1CCNC1
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
HO-
O.CN(C)C=O
0
2
CCOC(=O)N1CCC2C(C1)c1cccc3c1N2CC(C)N3C(=O)OCC.O=C1CCC(=O)N1Br>O.CN(C)C=O>CCOC(=O)N1CCC2C(C1)c1cc(Br)cc3c1N2CC(C)N3C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c991ff4f0ffe4caf906b891778ebccf7
CCOC(=O)N1CCC2C(C1)c1cc(Br)cc3c1N2CC(C)N3C(=O)OCC.OB(O)c1ccc(Cl)cc1Cl>>CCOC(=O)N1CCC2C(C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CC(C)N3C(=O)OCC
BrC=1C=C2C=3N(CC(N(C3C1)C(=O)OCC)C)C1C2CN(CC1)C(=O)OCC.ClC1=C(C=CC(=C1)Cl)B(O)O.C(=O)([O-])[O-].[Na+].[Na+]>>ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CC(N(C3C1)C(=O)OCC)C)C1C2CN(CC1)C(=O)OCC
Br[c:14]1[cH:13][c:12]2[c:25]3[c:24]([cH:23]1)[N:30]([C:31](=[O:32])[O:33][CH2:34][CH3:35])[CH:28]([CH3:29])[CH2:27][N:26]3[CH:9]1[CH2:8][CH2:7][N:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:11][CH:10]12.OB(O)[c:15]1[cH:16][cH:17][c:18]([Cl:19])[cH:20][c:21]1[Cl:22]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]1[CH2:7][CH2:8][CH...
CCOC(=O)N1CCC2C(C1)c1cc(Br)cc3c1N2CC(C)N3C(=O)OCC.OB(O)c1ccc(Cl)cc1Cl
CCOC(=O)N1CCC2C(C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CC(C)N3C(=O)OCC
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
CN(C)C=O.C(C)(=O)OCC
C-C Coupling
Suzuki coupling with boronic acids
76aadca826c052e8dd2b039b6a96f64b12ed2617c87c7ce270bedff0e0cd0dce
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cc3c4c(c2)C2CNCCC2N4CCN3)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]-[#7:6].O-B(-O)-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:10](-[Cl;D1;H0:11]):[c:12]>>[#7:6]-[c:5]:[c:4]:[c;H0;D3;+0:1](-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:10](-[Cl;D1;H0:11]):[c:12]):[c:2]:[c:3]
29
[{"value": 29.0, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CC(N(C3C1)C(=O)OCC)C)C1C2CN(CC1)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 26.3, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CC(N(C3C1)C(=O)OCC)C)C1C2CN(CC1)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
16
HOUR
To a solution of diethyl 5-bromo-2-methyl-6b,9,10,10a-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-3,8(2H,7H)-dicarboxylate (100 mg, 0.22 mmol) in DMF (10 mL) was added 2,4-dichlorophenyl boronic acid (63 mg, 0.33 mmol) and Na2CO3 (58 mg, 0.55 mmo, in 0.4 mL of H2O). The mixture was degassed with a strea...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2.c1ccccc1
c1ccccc1.c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1ccccc1.c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
HBr.B
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.CN(C)C=O.C(C)(=O)OCC
100
16
CCOC(=O)N1CCC2C(C1)c1cc(Br)cc3c1N2CC(C)N3C(=O)OCC.OB(O)c1ccc(Cl)cc1Cl>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.CN(C)C=O.C(C)(=O)OCC>CCOC(=O)N1CCC2C(C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CC(C)N3C(=O...
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-45ef0f63e0104c3c9bf0c39e4e78f987
CCOC(=O)N1CCC2C(C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CC(C)N3C(=O)OCC>>CC1CN2c3c(cc(-c4ccc(Cl)cc4Cl)cc3C3CNCCC32)N1
ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CC(N(C3C1)C(=O)OCC)C)C1C2CN(CC1)C(=O)OCC.[OH-].[K+]>>ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CC(NC3C1)C)C1C2CNCC1
CCOC(=O)[N:21]1[CH2:20][CH:19]2[c:18]3[c:5]4[c:6]([cH:7][c:8](-[c:9]5[cH:10][cH:11][c:12]([Cl:13])[cH:14][c:15]5[Cl:16])[cH:17]3)[N:25](C(=O)OCC)[CH:2]([CH3:1])[CH2:3][N:4]4[CH:24]2[CH2:23][CH2:22]1>>[CH3:1][CH:2]1[CH2:3][N:4]2[c:5]3[c:6]([cH:7][c:8](-[c:9]4[cH:10][cH:11][c:12]([Cl:13])[cH:14][c:15]4[Cl:16])[cH:17][c:1...
CCOC(=O)N1CCC2C(C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CC(C)N3C(=O)OCC
CC1CN2c3c(cc(-c4ccc(Cl)cc4Cl)cc3C3CNCCC32)N1
null
null
CCCCO.C(C)(=O)OCC
Reduction
OtherReaction
104ec19fce083dc1b862e57e6722f6d681cd1e46542715fa1d289f1df1fa3f44
4d54a9a4b5d62ab51cee46634e0429ca8b96a7950e75c860eb5742c8bca2fbcf
c1ccc(-c2cc3c4c(c2)C2CNCCC2N4CCN3)cc1
C-C-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5].C-C-O-C(=O)-[N;H0;D3;+0:6]1-[C:7](-[C;D1;H3:8])-[C:9]-[#7:10]-[c:11]:[c:12]-1:[c:13]>>[C;D1;H3:8]-[C:7]1-[C:9]-[#7:10]-[c:11]:[c:12](:[c:13])-[NH;D2;+0:6]-1.[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
45
[{"value": 45.0, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CC(NC3C1)C)C1C2CNCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 44.5, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=C2C=3N(CC(NC3C1)C)C1C2CNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
120
CELSIUS
16
HOUR
To a solution of diethyl 5-(2,4-dichlorophenyl)-2-methyl-6b,9,10,10a-tetrahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-3,8(2H,7H)-dicarboxylate (30 mg, 0.06 mmol) in 10 mL of n-BuOH was added KOH (33 mg, 0.6 mmol) and stirred at 120° C. for 16 h. The reaction was allowed to cool to ambient temperature and was...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Carbamic ester.Ether.Ether
Secondary amine.Secondary amine
c1cc2c3c(c1)C1C[NH]CCC1N3CC[NH]2
c1cc2c3c(c1)C1CNCCC1N3CCN2
c1ccccc1.c1cc2c3c(c1)C1CNCCC1N3CCN2
HO-
CCCCO.C(C)(=O)OCC
120
16
CCOC(=O)N1CCC2C(C1)c1cc(-c3ccc(Cl)cc3Cl)cc3c1N2CC(C)N3C(=O)OCC>CCCCO.C(C)(=O)OCC>CC1CN2c3c(cc(-c4ccc(Cl)cc4Cl)cc3C3CNCCC32)N1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ee37b3bbe8884342a72654bff4d2cc0e
Fc1ccccc1[CH2][Zn+].O=C(Cl)C1CCCCC1>>O=C(Cc1ccccc1F)C1CCCCC1
[Cl-].FC1=C(C[Zn+])C=CC=C1.C1(CCCCC1)C(=O)Cl>>FC1=C(CC(=O)C2CCCCC2)C=CC=C1
[Zn+][CH2:3][c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[F:10].Cl[C:2](=[O:1])[CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1>>[O:1]=[C:2]([CH2:3][c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[F:10])[CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1
Fc1ccccc1[CH2][Zn+].O=C(Cl)C1CCCCC1
O=C(Cc1ccccc1F)C1CCCCC1
null
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
null
C-C Coupling
OtherReaction
e0a45010daec094b0d5e8e4fbe0fbbb99cf9610754539ead723b25846a3ea8fc
fe2a4a0dfbb5b71b9a065e092364c64b22b4eb1ad4d6ba2a1e8edc9d31fce3e4
O=C(Cc1ccccc1)C1CCCCC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5].[Zn+]-[CH2;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH2;D2;+0:6]-[c:7](:[c:8]):[c:9])-[C:5]
null
[]
0
CELSIUS
null
null
To a mixture of 36 ml of 2-fluorobenzylzinc chloride (0.5 M sol. in tetrahydrofuran) and 0.008 g of dichlorobis(triphenylphosphine)palladium(II) stirred at 0° C. was added dropwise via a syringe 2.14 ml of cyclohexanecarbonyl chloride. Afterwards, the reaction mixture was stirred at r.t. for 4 h, quenched with an aqueo...
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Ketone
null
null
c1ccccc1.C1CCCCC1
Zn
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
0
null
Fc1ccccc1[CH2][Zn+].O=C(Cl)C1CCCCC1>Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl>O=C(Cc1ccccc1F)C1CCCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-77ac6db584834c1f8375001625f5f875
O=C(Cl)C1CCCCC1.[Zn+][CH2]c1ccccc1>>O=C(Cc1ccccc1)C1CCCCC1
C1(CCCCC1)C(=O)Cl.[Br-].C(C1=CC=CC=C1)[Zn+]>>C1(CCCCC1)C(=O)CC1=CC=CC=C1
Cl[C:2](=[O:1])[CH:10]1[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]1.[Zn+][CH2:3][c:4]1[cH:5][cH:6][cH:7][cH:8][cH:9]1>>[O:1]=[C:2]([CH2:3][c:4]1[cH:5][cH:6][cH:7][cH:8][cH:9]1)[CH:10]1[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]1
O=C(Cl)C1CCCCC1.[Zn+][CH2]c1ccccc1
O=C(Cc1ccccc1)C1CCCCC1
null
null
O1CCCC1
C-C Coupling
OtherReaction
e0a45010daec094b0d5e8e4fbe0fbbb99cf9610754539ead723b25846a3ea8fc
fe2a4a0dfbb5b71b9a065e092364c64b22b4eb1ad4d6ba2a1e8edc9d31fce3e4
O=C(Cc1ccccc1)C1CCCCC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5].[Zn+]-[CH2;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH2;D2;+0:6]-[c:7](:[c:8]):[c:9])-[C:5]
52
[{"value": 52.0, "product": "C1(CCCCC1)C(=O)CC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
To a solution of 11 ml of 0.5 M solution of benzyl zinc bromide in anhydrous tetrahydrofuran were added at 0° C. 5 mg of bis-triphenylphospinepalladium dichloride and 0.66 ml of cyclohexanecarbonyl chloride. The mixture was stirred at r.t. for 1.5 h, quenched with a saturated solution of ammonium chloride and extracted...
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Ketone
null
null
c1ccccc1.C1CCCCC1
Zn
O1CCCC1
null
1.5
O=C(Cl)C1CCCCC1.[Zn+][CH2]c1ccccc1>O1CCCC1>O=C(Cc1ccccc1)C1CCCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0f065b34f4cd4e0a9ab3bbb53d94a9e4
CCOC(CC(C(=O)C1CCCCC1)c1ccccc1)OCC>>O=CCC(C(=O)C1CCCCC1)c1ccccc1
C(C)OC(CC(C(=O)C1CCCCC1)C1=CC=CC=C1)OCC>>C1(CCCCC1)C(C(CC=O)C1=CC=CC=C1)=O
CCO[CH:2]([O:1]CC)[CH2:3][CH:4]([C:5](=[O:6])[CH:7]1[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1)[c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1>>[O:1]=[CH:2][CH2:3][CH:4]([C:5](=[O:6])[CH:7]1[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1)[c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1
CCOC(CC(C(=O)C1CCCCC1)c1ccccc1)OCC
O=CCC(C(=O)C1CCCCC1)c1ccccc1
null
null
Cl.CC(=O)C
Miscellaneous
Acetal hydrolysis to aldehyde
2c5baf4818f438d514702dbb9f9a64f069b67040aebce8bef29fab8232955599
84d5a69453aa750f462aa94a6bf2116fc17c5d88a9619aaa9eefb74b0c09848d
O=C(Cc1ccccc1)C1CCCCC1
C-C-O-[CH;D3;+0:1](-[C:2]-[C:3]-[C:4]=[O;D1;H0:5])-[O;H0;D2;+0:6]-C-C>>[O;D1;H0:5]=[C:4]-[C:3]-[C:2]-[CH;D2;+0:1]=[O;H0;D1;+0:6]
100
[{"value": 100.0, "product": "C1(CCCCC1)C(C(CC=O)C1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.6, "product": "C1(CCCCC1)C(C(CC=O)C1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of 1.17 g of Compound 5b in 10 ml of acetone and 22.1 ml of 2N HCl was stirred at r.t. for 5 h. After overnight resting, the aqueous layer was extracted with EtOAc. The collected organic layers were washed with water, dried (Na2SO4) and the solvent was evaporated under vacuum to give 0.84 g (100%) of the tit...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Aldehyde
null
null
C1CCCCC1.c1ccccc1
HO-
Cl.CC(=O)C
null
8
CCOC(CC(C(=O)C1CCCCC1)c1ccccc1)OCC>Cl.CC(=O)C>O=CCC(C(=O)C1CCCCC1)c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6dd37b3ea8d64736b1e8a46281be986b
COc1ccccc1N1CCNCC1.O=CCC(C(=O)C1CCCCC1)c1ccccc1>>COc1ccccc1N1CCN(CCC(C(=O)C2CCCCC2)c2ccccc2)CC1
C1(CCCCC1)C(C(CC=O)C1=CC=CC=C1)=O.COC1=C(C=CC=C1)N1CCNCC1.C(C)(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+].C(C)(=O)O>>C1(CCCCC1)C(C(CCN1CCN(CC1)C1=C(C=CC=C1)OC)C1=CC=CC=C1)=O
[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[N:9]1[CH2:10][CH2:11][NH:12][CH2:30][CH2:31]1.O=[CH:13][CH2:14][CH:15]([C:16](=[O:17])[CH:18]1[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]1)[c:24]1[cH:25][cH:26][cH:27][cH:28][cH:29]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[N:9]1[CH2:10][CH2:11][N:12]([CH2:13][CH2:...
COc1ccccc1N1CCNCC1.O=CCC(C(=O)C1CCCCC1)c1ccccc1
COc1ccccc1N1CCN(CCC(C(=O)C2CCCCC2)c2ccccc2)CC1
null
null
ClCCl
Heteroatom Alkylation and Arylation
reductive amination
66e6667395903ee1c54d8aecc784ece1bccbdcbc9661ebcae0e6a980f9380640
2d03f38884b1fbb0c0d6e6f2de31afb25102fec87f347c3a123e064c1bfef0ad
O=C(C1CCCCC1)C(CCN1CCN(c2ccccc2)CC1)c1ccccc1
O=[CH;D2;+0:1]-[C:2]-[C:3]-[C:4]=[O;D1;H0:5].[#7:6]1-[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]-1>>[O;D1;H0:5]=[C:4]-[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:9]1-[C:8]-[C:7]-[#7:6]-[C:11]-[C:10]-1
100.3
[{"value": 99.0, "product": "C1(CCCCC1)C(C(CCN1CCN(CC1)C1=C(C=CC=C1)OC)C1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 100.3, "product": "C1(CCCCC1)C(C(CCN1CCN(CC1)C1=C(C=CC=C1)OC)C1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
To a solution of 0.84 g of Compound 5c and 1.19 g of 1-(2-methoxyphenyl)-piperazine in 30 ml of dichloromethane, 1.48 g of sodium triacetoxyborohydride and 0.98 ml of acetic acid were added and the resulting mixture was stirred at r.t. for 5 h. After overnight resting, the organic layer was washed with excess of 1M NaO...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine
Tertiary amine
C1C[NH]CCN1
C1C[NH]CC[NH]1
c1ccccc1.C1C[NH]CC[NH]1.C1CCCCC1.c1ccccc1
Other
ClCCl
null
5
COc1ccccc1N1CCNCC1.O=CCC(C(=O)C1CCCCC1)c1ccccc1>ClCCl>COc1ccccc1N1CCN(CCC(C(=O)C2CCCCC2)c2ccccc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a2c6d18735294db9a4cec801c19b3d02
COc1ccccc1N1CCN(CCC(C(=O)C2CCCCC2)c2ccccc2)CC1>>COc1ccccc1N1CCN(CCC(c2ccccc2)C(O)C2CCCCC2)CC1
C1(CCCCC1)C(C(CCN1CCN(CC1)C1=C(C=CC=C1)OC)C1=CC=CC=C1)=O.[H-].C(C(C)C)[Al+]CC(C)C>>C1(CCCCC1)C(C(CCN1CCN(CC1)C1=C(C=CC=C1)OC)C1=CC=CC=C1)O
[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[N:9]1[CH2:10][CH2:11][N:12]([CH2:13][CH2:14][CH:15]([c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[C:22](=[O:23])[CH:24]2[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29]2)[CH2:30][CH2:31]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[N:9]1[CH2:10][CH2:11][N:12]([CH2:13][CH2:1...
COc1ccccc1N1CCN(CCC(C(=O)C2CCCCC2)c2ccccc2)CC1
COc1ccccc1N1CCN(CCC(c2ccccc2)C(O)C2CCCCC2)CC1
null
null
ClCCl.C1(=CC=CC=C1)C
Reduction
Reduction of ketone to secondary alcohol
02790ac194d8bf7ccb13d6247c59412024d87f77d2c906ef7804f021f57d5070
1bd3cd74b454139c0a0068ac0135836499926b274bff569df163210c6c944a89
c1ccc(C(CCN2CCN(c3ccccc3)CC2)CC2CCCCC2)cc1
[C:1]-[C:2](-[c:3])-[C;H0;D3;+0:4](=[O;H0;D1;+0:5])-[C:6](-[C:7])-[C:8]>>[C:1]-[C:2](-[c:3])-[CH;D3;+0:4](-[OH;D1;+0:5])-[C:6](-[C:7])-[C:8]
87.2
[{"value": 80.0, "product": "C1(CCCCC1)C(C(CCN1CCN(CC1)C1=C(C=CC=C1)OC)C1=CC=CC=C1)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.2, "product": "C1(CCCCC1)C(C(CCN1CCN(CC1)C1=C(C=CC=C1)OC)C1=CC=CC=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
1
HOUR
Into a solution of 1.21 g of Compound 5d in 60 ml of dichloromethane at −78° C., was dropped 11.5 ml of 1 M solution of diisobutylaluminum hydride (DIBAL-H) in toluene. The mixture was stirred at −78° C. for 1 h, quenched at 40° C. with a saturated aqueous solution of NH4Cl and extracted with chloroform. The collected ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
null
null
c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1.C1CCCCC1
null
ClCCl.C1(=CC=CC=C1)C
-78
1
COc1ccccc1N1CCN(CCC(C(=O)C2CCCCC2)c2ccccc2)CC1>ClCCl.C1(=CC=CC=C1)C>COc1ccccc1N1CCN(CCC(c2ccccc2)C(O)C2CCCCC2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fbaa14d6e4c243d89586713fa1c24c59
O=P(Cl)(Cl)Cl.O=c1cnc2c([nH]1)CCCC2>>Clc1cnc2c(n1)CCCC2
N1C(C=NC=2CCCCC12)=O.P(=O)(Cl)(Cl)Cl>>ClC1=NC=2CCCCC2N=C1
O=P(Cl)(Cl)[Cl:1].O=[c:2]1[cH:3][n:4][c:5]2[c:6]([nH:7]1)[CH2:8][CH2:9][CH2:10][CH2:11]2>>[Cl:1][c:2]1[cH:3][n:4][c:5]2[c:6]([n:7]1)[CH2:8][CH2:9][CH2:10][CH2:11]2
O=P(Cl)(Cl)Cl.O=c1cnc2c([nH]1)CCCC2
Clc1cnc2c(n1)CCCC2
null
null
null
Functional Group Interconversion
OtherReaction
1282c63ec158ab45b09d1c279ad07e86c94206a6cfce12271ada1f3c04d3f379
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1cnc2c(n1)CCCC2
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].O=[c;H0;D3;+0:2]1:[c:3]:[#7;a:4]:[c:5](:[c:6](:[nH;D2;+0:7]:1)-[C:8])-[C:9]>>[C:9]-[c:5]1:[#7;a:4]:[c:3]:[c;H0;D3;+0:2](-[Cl;H0;D1;+0:1]):[n;H0;D2;+0:7]:[c:6]:1-[C:8]
86
[{"value": 86.0, "product": "ClC1=NC=2CCCCC2N=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 5,6,7,8-tetrahydro-2(1H)-quinoxalinone in phosphoryl chloride (200 ml) was stirred and refluxed for 3 hours. The solvent was evaporated. The residue was taken up in ice and CH2Cl2. The mixture was basified with NH4OH. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated, ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1cnc2c(n1)CCCC2
c1cnc2c(n1)CCCC2
c1cnc2c(n1)CCCC2
HCl
null
null
null
O=P(Cl)(Cl)Cl.O=c1cnc2c([nH]1)CCCC2>>Clc1cnc2c(n1)CCCC2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a0f99a5dfa9a45848a8856bf58a18c6e
CC(=O)C(C)=O.CCOC(=O)c1cccc(N)c1N>>CCOC(=O)c1cccc2nc(C)c(C)nc12
C(=O)([O-])[O-].[K+].[K+].CC(C(C)=O)=O.S(=O)(=O)([O-])S(=O)[O-].[Na+].[Na+].NC1=C(C(=O)OCC)C=CC=C1N>>CC1=NC=2C=CC=C(C2N=C1C)C(=O)OCC
O=[C:12]([CH3:13])[C:14](=O)[CH3:15].[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][cH:9][c:10]([NH2:11])[c:17]1[NH2:16]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][cH:9][c:10]2[n:11][c:12]([CH3:13])[c:14]([CH3:15])[n:16][c:17]12
CC(=O)C(C)=O.CCOC(=O)c1cccc(N)c1N
CCOC(=O)c1cccc2nc(C)c(C)nc12
null
null
O
Aromatic Heterocycle Formation
OtherReaction
80ad7d4b359f2683f57c053570cf5c6857c4f32e8ec9869e4f38f79c70cafc8c
d53d864708a4cd37c2fe33ca368498c017ca81ee7d694ff92f9c935efef6bc9e
c1ccc2nccnc2c1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[C;H0;D3;+0:3](=O)-[C;D1;H3:4].[#8:5]-[C:6](=[O;D1;H0:7])-[c:8]:[c:9](-[NH2;D1;+0:10]):[c:11](-[NH2;D1;+0:12]):[c:13]>>[#8:5]-[C:6](=[O;D1;H0:7])-[c:8]:[c:9]1:[n;H0;D2;+0:10]:[c;H0;D3;+0:3](-[C;D1;H3:4]):[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D2;+0:12]:[c:11]:1:[c:13]
67.2
[{"value": 67.0, "product": "CC1=NC=2C=CC=C(C2N=C1C)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 67.2, "product": "CC1=NC=2C=CC=C(C2N=C1C)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
12
HOUR
2,3-Butanedione (0.0776 mol) was added at room temperature to a solution of sodium pyrosulfite (0.1 mol) in water (75 ml). The mixture was heated to 70° C. and then added to a solution of ethyl 2,3-diaminobenzoate (0.0776 mol) in water (75 ml). The mixture was stirred at 100° C. for 12 hours, cooled, basified with K2CO...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone.Primary amine.Primary amine
null
c1ccccc1
c1ccc2nccnc2c1
c1ccc2nccnc2c1
HO-
O
70
12
CC(=O)C(C)=O.CCOC(=O)c1cccc(N)c1N>O>CCOC(=O)c1cccc2nc(C)c(C)nc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-60ac4e1b4f544e8ba45a2727dbe686f7
CN(C)C=O.Cc1ccc2cccc(Br)c2n1>>Cc1ccc2cccc(C=O)c2n1
[NH4+].[Cl-].CN(C)C=O.BrC=1C=CC=C2C=CC(=NC12)C.[NH4+].[Cl-].C(CCC)[Li].CCCCCC>>CC1=NC2=C(C=CC=C2C=C1)C=O
CN(C)[CH:10]=[O:11].Br[c:9]1[cH:8][cH:7][cH:6][c:5]2[cH:4][cH:3][c:2]([CH3:1])[n:13][c:12]21>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[cH:6][cH:7][cH:8][c:9]([CH:10]=[O:11])[c:12]2[n:13]1
CN(C)C=O.Cc1ccc2cccc(Br)c2n1
Cc1ccc2cccc(C=O)c2n1
null
null
O1CCCC1.C(C)OCC.C(C)O
C-C Coupling
Bouveault aldehyde synthesis
6b2ee0acc9e3f7a1d11938f6d9a15d00e6e8ead5dccbbdb0a71f0ce23f9e361d
afd09ced98f25d311f21cc04ba6a50fe7e5516de47e17484683ded13d323b1b2
c1ccc2ncccc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].C-N(-C)-[CH;D2;+0:8]=[O;D1;H0:9]>>[O;D1;H0:9]=[CH;D2;+0:8]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]
129.8
[{"value": 100.0, "product": "CC1=NC2=C(C=CC=C2C=C1)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 129.8, "product": "CC1=NC2=C(C=CC=C2C=C1)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-70
CELSIUS
30
MINUTE
8-Bromo-2-methylquinoline (0.0675 mol) was added portionwise at −70° C. under N2 flow to a mixture of a solution of butyllithium in hexane (1.6M) (0.135 mol) in tetrahydrofuran (300 ml) and diethyl ether (300 ml). The mixture was stirred for 30 minutes. A solution of DMF (0.405 mol) in tetrahydrofuran (100 ml) was adde...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tertiary amide
Aldehyde
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HBr
O1CCCC1.C(C)OCC.C(C)O
-70
0.5
CN(C)C=O.Cc1ccc2cccc(Br)c2n1>O1CCCC1.C(C)OCC.C(C)O>Cc1ccc2cccc(C=O)c2n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e14ca53373f947628d9a61d018702f84
COc1cc2ccccc2nc1C>>COc1cc2c(nc1C)CCCC2
COC=1C(=NC2=CC=CC=C2C1)C.[H][H]>>COC=1C(=NC=2CCCCC2C1)C
[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([n:7][c:8]1[CH3:9])[cH:10][cH:11][cH:12][cH:13]2>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([n:7][c:8]1[CH3:9])[CH2:10][CH2:11][CH2:12][CH2:13]2
COc1cc2ccccc2nc1C
COc1cc2c(nc1C)CCCC2
null
[Pd]
FC(C(=O)O)(F)F
Reduction
OtherReaction
9304ef4b145871f015039f0f87a526880ef1ccc35aa5ca268466778d480e3cfe
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1cnc2c(c1)CCCC2
[c:1]:[c:2]1:[cH;D2;+0:3]:[cH;D2;+0:4]:[cH;D2;+0:5]:[cH;D2;+0:6]:[c:7]:1:[#7;a:8]:[c:9]>>[c:1]:[c:2]1:[c:7](:[#7;a:8]:[c:9])-[CH2;D2;+0:6]-[CH2;D2;+0:5]-[CH2;D2;+0:4]-[CH2;D2;+0:3]-1
99.6
[{"value": 99.6, "product": "COC=1C(=NC=2CCCCC2C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 3-methoxy-2-methylquinoline (0.081 mol) in trifluoro-acetic acid (150 ml) was hydrogenated at room temperature under a 34 bar pressure for 48 hours with palladium on activated carbon (2 g) as a catalyst. After uptake of hydrogen (2 equiv.), the catalyst was filtered through celite and washed with H2O. The ...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2ncccc2c1
c1cnc2c(c1)CCCC2
c1cnc2c(c1)CCCC2
null
[Pd].FC(C(=O)O)(F)F
null
null
COc1cc2ccccc2nc1C>[Pd].FC(C(=O)O)(F)F>COc1cc2c(nc1C)CCCC2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ec5c825169ea4d32846c8d18ec613a69
BrP(Br)Br.Cc1ccc2c(n1)C(O)CCC2>>Cc1ccc2c(n1)C(Br)CCC2
P(Br)(Br)Br.CC1=NC=2C(CCCC2C=C1)O.CC1=NC=2C(CCCC2C=C1)O.[OH-].[Na+]>>BrC1CCCC=2C=CC(=NC12)C
BrP(Br)[Br:9].O[CH:8]1[c:6]2[c:5]([cH:4][cH:3][c:2]([CH3:1])[n:7]2)[CH2:12][CH2:11][CH2:10]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[c:6]([n:7]1)[CH:8]([Br:9])[CH2:10][CH2:11][CH2:12]2
BrP(Br)Br.Cc1ccc2c(n1)C(O)CCC2
Cc1ccc2c(n1)C(Br)CCC2
null
null
C1(=CC=CC=C1)C
Functional Group Interconversion
OtherReaction
4eb07b06ca6bf965c8defd9b5553b478ca022fffadf84ff14f680b94d0889668
495868b18ac37eabad313a8861412e57f019fb3569a2b2e50afa3ee29413ec02
c1cnc2c(c1)CCCC2
Br-P(-Br)-[Br;H0;D1;+0:1].O-[CH;D3;+0:2](-[C:3]-[C:4])-[c:5](:[c:6]):[#7;a:7]:[c:8]>>[Br;H0;D1;+0:1]-[CH;D3;+0:2](-[C:3]-[C:4])-[c:5](:[c:6]):[#7;a:7]:[c:8]
84.2
[{"value": 29.0, "product": "BrC1CCCC=2C=CC(=NC12)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.2, "product": "BrC1CCCC=2C=CC(=NC12)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Phosphorus tribromide (0.0105 mol) was added dropwise at 0° C./5° C. under N2 flow to a mixture of (±)-5,6,7,8-tetrahydro-2-methyl-8-quinolinol (intermediate 17) (0.03 mol) in toluene (20 ml). The mixture was brought to room temperature and stirred at room temperature overnight. Ice water was added. The mixture was bas...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Secondary halide
c1cnc2c(c1)CCCC2
c1cnc2c(c1)CCCC2
c1cnc2c(c1)CCCC2
HBr
C1(=CC=CC=C1)C
null
8
BrP(Br)Br.Cc1ccc2c(n1)C(O)CCC2>C1(=CC=CC=C1)C>Cc1ccc2c(n1)C(Br)CCC2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a51d87559ef241039e7ebf5f2a91a9df
O=CNc1cccc2cccnc12.O=[N+]([O-])c1ccccc1Cl>>O=[N+]([O-])c1ccccc1Nc1cccc2cccnc12
ClC1=C(C=CC=C1)[N+](=O)[O-].N1=CC=CC2=CC=CC(=C12)NC=O.[H-].[Na+].O>>[N+](=O)([O-])C1=C(C=CC=C1)NC=1C=CC=C2C=CC=NC12
O=C[NH:10][c:11]1[cH:12][cH:13][cH:14][c:15]2[cH:16][cH:17][cH:18][n:19][c:20]12.Cl[c:9]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][cH:6][cH:7][cH:8]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[NH:10][c:11]1[cH:12][cH:13][cH:14][c:15]2[cH:16][cH:17][cH:18][n:19][c:20]12
O=CNc1cccc2cccnc12.O=[N+]([O-])c1ccccc1Cl
O=[N+]([O-])c1ccccc1Nc1cccc2cccnc12
null
null
CN(C)C=O
Functional Group Addition
OtherReaction
1821c4c8060175bf390d94295fd88f196f59741d36e2f9631c86d4ef54fe9389
1d196ba5d3235d0f70196a5df15f7e51895b680a6c5e6ae9c7e22f63a0e77a26
c1ccc(Nc2cccc3cccnc23)cc1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].O=C-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10](:[c:11]):[#7;a:12]:[c:13]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10](:[c:11]):[#7;a:12]:[c:13]):[c:2]:[c:3]
21.2
[{"value": 21.0, "product": "[N+](=O)([O-])C1=C(C=CC=C1)NC=1C=CC=C2C=CC=NC12", "details": "PERCENTYIELD", "is_desired": false}, {"value": 21.2, "product": "[N+](=O)([O-])C1=C(C=CC=C1)NC=1C=CC=C2C=CC=NC12", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A dispersion of sodium hydride in mineral oil (0.261 mol) was added portionwise at room temperature under N2 flow to a mixture of N-8-quinolinylformamide (0.174 mol) in DMF (500 ml). The mixture was stirred at room temperature for 1 hour. A solution of 1-chloro-2-nitrobenzene (0.53 mol) in DMF (200 ml) was added dropwi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amide
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccc2ncccc2c1
HCl
CN(C)C=O
null
1
O=CNc1cccc2cccnc12.O=[N+]([O-])c1ccccc1Cl>CN(C)C=O>O=[N+]([O-])c1ccccc1Nc1cccc2cccnc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9ca8affbf2c845d8a5ea54ffd2219358
CCOC(OCC)OCC.O=Cc1cccc2cccnc12>>CCOC(OCC)c1cccc2cccnc12
C(=O)([O-])[O-].[K+].[K+].N1=CC=CC2=CC=CC(=C12)C=O.C(C)OC(OCC)OCC.CC1=CC=C(C=C1)S(=O)(=O)O>>C(C)OC(C=1C=CC=C2C=CC=NC12)OCC
CCOC(O[CH2:2][CH3:1])[O:5][CH2:6][CH3:7].[O:3]=[CH:4][c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][cH:14][cH:15][n:16][c:17]12>>[CH3:1][CH2:2][O:3][CH:4]([O:5][CH2:6][CH3:7])[c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][cH:14][cH:15][n:16][c:17]12
CCOC(OCC)OCC.O=Cc1cccc2cccnc12
CCOC(OCC)c1cccc2cccnc12
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
fcd88c7abf874cee525e2d08e112aab4759e77ad93b33f36b8306c7913ea31c2
11306b4f2dea9cefbc3d550c8afb389271a44b7cc69c06172e6b191dd38b2284
c1ccc2ncccc2c1
C-C-O-C(-O-[CH2;D2;+0:1]-[C;D1;H3:2])-[O;H0;D2;+0:3]-[C:4]-[C;D1;H3:5].[O;H0;D1;+0:6]=[CH;D2;+0:7]-[c:8](:[c:9]):[c:10](:[c:11]):[#7;a:12]:[c:13]>>[C;D1;H3:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[CH;D3;+0:7](-[O;H0;D2;+0:3]-[C:4]-[C;D1;H3:5])-[c:8](:[c:9]):[c:10](:[c:11]):[#7;a:12]:[c:13]
84.6
[{"value": 80.0, "product": "C(C)OC(C=1C=CC=C2C=CC=NC12)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.6, "product": "C(C)OC(C=1C=CC=C2C=CC=NC12)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 8-quinolinecarboxaldehyde (0.248 mol), triethoxymethane (0.4464 mol) and 4-methylbenzenesulfonic acid (4 g) in ethanol (250 ml) was stirred and refluxed for 1 hour, brought to room temperature, poured out into K2CO3 10% and extracted with EtOAc. The organic layer was separated, dried (MgSO4), filtered and ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ether.Ether.Ether
Ether.Ether
null
null
c1ccc2ncccc2c1
HO-
C(C)O
null
null
CCOC(OCC)OCC.O=Cc1cccc2cccnc12>C(C)O>CCOC(OCC)c1cccc2cccnc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3d5a2eebd5444a19a9d7ea089a49bc03
CCO.Cc1ccc(S(=O)(=O)O)cc1.O=Cc1ccc2ccccc2n1>>CCOC(OCC)c1ccc2ccccc2n1
N1=C(C=CC2=CC=CC=C12)C=O.CC1=CC=C(C=C1)S(=O)(=O)O.C(C)O>>C(C)OC(C1=NC2=CC=CC=C2C=C1)OCC
[OH:5][CH2:6][CH3:7].Cc1ccc(S(=O)(=O)O)[cH:1][cH:2]1.[O:3]=[CH:4][c:8]1[cH:9][cH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[n:17]1>>[CH3:1][CH2:2][O:3][CH:4]([O:5][CH2:6][CH3:7])[c:8]1[cH:9][cH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[n:17]1
CCO.Cc1ccc(S(=O)(=O)O)cc1.O=Cc1ccc2ccccc2n1
CCOC(OCC)c1ccc2ccccc2n1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
a41db0c1ee2b64dae978f85650c33aa8b5de4efe5372b010d3f57b5638a2f80a
0d641fbcfd93c2628ed6fe4905bfe9d21a8c042d9bd5e63f31d12bc8ee448be4
c1ccc2ncccc2c1
C-c1:[cH;D2;+0:1]:[cH;D2;+0:2]:c(-S(-O)(=O)=O):c:c:1.[C;D1;H3:3]-[C:4]-[OH;D1;+0:5].[O;H0;D1;+0:6]=[CH;D2;+0:7]-[c:8](:[c:9]):[#7;a:10]:[c:11]>>[C;D1;H3:3]-[C:4]-[O;H0;D2;+0:5]-[CH;D3;+0:7](-[O;H0;D2;+0:6]-[CH2;D2;+0:1]-[CH3;D1;+0:2])-[c:8](:[c:9]):[#7;a:10]:[c:11]
null
[]
null
null
null
null
A mixture of 2-quinolinecarboxaldehyde (0.08 mol) and 4-methylbenzenesulfonic acid (0.25 g) in ethanol (100 ml) was stirred and refluxed for 48 hours and brought to room temperature. The reaction was carried out again using the same quantities. The mixtures were combined. The solvent was evaporated. The residue was tak...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Aldehyde.Primary alcohol
Ether.Ether
c1ccccc1
null
c1ccc2ncccc2c1
TsOH.HO-
null
null
null
CCO.Cc1ccc(S(=O)(=O)O)cc1.O=Cc1ccc2ccccc2n1>>CCOC(OCC)c1ccc2ccccc2n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d01099ba7a7745ea9ec56d0be6ad390a
CC(C)C(CO)N(C(=O)O)C(C)(C)C.Cc1ccc(S(=O)(=O)Cl)cc1>>Cc1ccc(S(=O)(=O)OCC(NC(=O)OC(C)(C)C)C(C)C)cc1
CC1=CC=C(C=C1)S(=O)(=O)Cl.CC(C)(C)N(C(O)=O)C(C(C)C)CO.O>>CC1=CC=C(C=C1)S(=O)(=O)OCC(C(C)C)NC(OC(C)(C)C)=O
[OH:9][CH2:10][CH:11]([N:12]([C:13](=[O:14])[OH:15])[C:16]([CH3:17])([CH3:18])[CH3:19])[CH:20]([CH3:21])[CH3:22].Cl[S:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:24][cH:23]1)(=[O:7])=[O:8]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[O:9][CH2:10][CH:11]([NH:12][C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19]...
CC(C)C(CO)N(C(=O)O)C(C)(C)C.Cc1ccc(S(=O)(=O)Cl)cc1
Cc1ccc(S(=O)(=O)OCC(NC(=O)OC(C)(C)C)C(C)C)cc1
null
null
N1=CC=CC=C1
Protection
OtherReaction
db06ccc74404c99bedd0938c8e49fa1847f8469ffa2dc5725a343c45e4efbc6e
719bbcc3bcf5c95f3deccecbe2f76966ae2f47c5ebad05f7b7b9b81f1532a3c7
c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[C:7]-[C:8](-[C:9]-[OH;D1;+0:10])-[N;H0;D3;+0:11](-[C:12](=[O;D1;H0:13])-[OH;D1;+0:14])-[C;H0;D4;+0:15](-[C;D1;H3:16])(-[C;D1;H3:17])-[C;D1;H3:18]>>[C:7]-[C:8](-[C:9]-[O;H0;D2;+0:10]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6])-[NH;D2;...
123.4
[{"value": 68.0, "product": "CC1=CC=C(C=C1)S(=O)(=O)OCC(C(C)C)NC(OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 123.4, "product": "CC1=CC=C(C=C1)S(=O)(=O)OCC(C(C)C)NC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
10
CELSIUS
2
HOUR
4-Methylbenzenesulfonyl chloride (0.2222 mol) was added portionwise at 10° C. to a mixture of 1,1-dimethylethyl [1-(hydroxymethyl)-2-methylpropyl]carbamic acid (ester) (0.202 mol) in pyridine (65 ml). The mixture was stirred at 10° C. for 2 hours. H2O (75 ml) was added at 10° C. The precipitate was filtered off, washed...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Carbamic acid.Primary alcohol.Sulfonyl halide
Tosylate.Carbamic ester.Ether.Boc
null
null
c1ccccc1
HCl
N1=CC=CC=C1
10
2
CC(C)C(CO)N(C(=O)O)C(C)(C)C.Cc1ccc(S(=O)(=O)Cl)cc1>N1=CC=CC=C1>Cc1ccc(S(=O)(=O)OCC(NC(=O)OC(C)(C)C)C(C)C)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f06646f0255f405a83ee2f07535442db
CC(C)C(=O)CN1CCC(Nc2nc3ccccc3[nH]2)CC1>>CC(C)C(N)CN1CCC(Nc2nc3ccccc3[nH]2)CC1
N1C(=NC2=C1C=CC=C2)NC2CCN(CC2)CC(C(C)C)=O.C1(=CC=CC=C1)CN>>NC(CN1CCC(CC1)NC1=NC2=C(N1)C=CC=C2)C(C)C
O=[C:4]([CH:2]([CH3:1])[CH3:3])[CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([NH:11][c:12]2[n:13][c:14]3[cH:15][cH:16][cH:17][cH:18][c:19]3[nH:20]2)[CH2:21][CH2:22]1>>[CH3:1][CH:2]([CH3:3])[CH:4]([NH2:5])[CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([NH:11][c:12]2[n:13][c:14]3[cH:15][cH:16][cH:17][cH:18][c:19]3[nH:20]2)[CH2:21][CH2:22]1
CC(C)C(=O)CN1CCC(Nc2nc3ccccc3[nH]2)CC1
CC(C)C(N)CN1CCC(Nc2nc3ccccc3[nH]2)CC1
null
[Pd]
CO
Functional Group Interconversion
Mignonac reaction
14af499c4b742b1ab2135a986a4f7f4e6dda0ad50987736be8cf00d531c63192
2ef9e3e9915394571ec6196ff6ea06bca9f3dff8c6f6f43c81edc876014a94a5
c1ccc2[nH]c(NC3CCNCC3)nc2c1
O=[C;H0;D3;+0:1](-[C:2]-[#7:3])-[C:4](-[C;D1;H3:5])-[C;D1;H3:6]>>[#7:3]-[C:2]-[CH;D3;+0:1](-[N;D1;H2:7])-[C:4](-[C;D1;H3:5])-[C;D1;H3:6]
4.4
[{"value": 4.4, "product": "NC(CN1CCC(CC1)NC1=NC2=C(N1)C=CC=C2)C(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A mixture of 1-[4-(1H-benzimidazol-2-ylamino)-1-piperidinyl]-3-methyl-2-butanone (0.03 mol) and benzenemethanamine (0.09 mol) in methanol (200 ml) was hydrogenated at 40° C. under a 3 bar pressure for 48 hours with palladium on activated carbon (1.3 g) as a catalyst. After uptake of hydrogen, the catalyst was filtered ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary amine
null
null
C1CC[NH]CC1.c1ccc2[nH]cnc2c1
null
[Pd].CO
null
24
CC(C)C(=O)CN1CCC(Nc2nc3ccccc3[nH]2)CC1>[Pd].CO>CC(C)C(N)CN1CCC(Nc2nc3ccccc3[nH]2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1031a038c29a45a5bfb270ecacaba076
CC(C)C(=O)CN1CCC(Nc2nc3ccccc3n2-c2cccc3cccnc23)CC1>>CC(C)C(=O)CN1CCC(Nc2nc3ccccc3n2-c2cccc3c2NCCC3)CC1
N1=CC=CC2=CC=CC(=C12)N1C(=NC2=C1C=CC=C2)NC2CCN(CC2)CC(C(C)C)=O.C1(=CC=CC=C1)CN>>N1CCCC2=CC=CC(=C12)N1C(=NC2=C1C=CC=C2)NC2CCN(CC2)CC(C(C)C)=O
[CH3:1][CH:2]([CH3:3])[C:4](=[O:5])[CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([NH:11][c:12]2[n:13][c:14]3[cH:15][cH:16][cH:17][cH:18][c:19]3[n:20]2-[c:21]2[cH:22][cH:23][cH:24][c:25]3[c:26]2[n:27][cH:28][cH:29][cH:30]3)[CH2:31][CH2:32]1>>[CH3:1][CH:2]([CH3:3])[C:4](=[O:5])[CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([NH:11][c:12]2[n:13]...
CC(C)C(=O)CN1CCC(Nc2nc3ccccc3n2-c2cccc3cccnc23)CC1
CC(C)C(=O)CN1CCC(Nc2nc3ccccc3n2-c2cccc3c2NCCC3)CC1
null
[Pd]
CO
Reduction
OtherReaction
0f501d7f6563b973124f46b9ac99227bf4e9d23710ef3fe61283d96ce59150d0
2b7f370a519e29b4dede190aa36b37f30822496e32f2c8bfa9736e631bde52e2
c1cc2c(c(-n3c(NC4CCNCC4)nc4ccccc43)c1)NCCC2
[c:1]:[c:2]1:[n;H0;D2;+0:3]:[cH;D2;+0:4]:[cH;D2;+0:5]:[cH;D2;+0:6]:[c:7]:1:[c:8]>>[c:1]:[c:2]1:[c:7](:[c:8])-[CH2;D2;+0:6]-[CH2;D2;+0:5]-[CH2;D2;+0:4]-[NH;D2;+0:3]-1
27.1
[{"value": 27.1, "product": "N1CCCC2=CC=CC(=C12)N1C(=NC2=C1C=CC=C2)NC2CCN(CC2)CC(C(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A mixture of 1-[4-[[1-(8-quinolinyl)-1H-benzimidazol-2-yl]amino]1-piperidinyl]-3-methyl-2-butanone (0.0222 mol) and benzenemethanamine (0.0666 mol) in methanol (250 ml) was hydrogenated at 40° C. under a 3 bar pressure for 24 hours with palladium on activated carbon (1.5 g) as a catalyst. After uptake of hydrogen, the ...
10.6084/m9.figshare.5104873.v1
null
null
Secondary amine
c1ccc2ncccc2c1
c1ccc2c(c1)CCCN2
C1CC[NH]CC1.c1nc2ccccc2[nH]1.c1ccc2c(c1)CCCN2
null
[Pd].CO
null
24
CC(C)C(=O)CN1CCC(Nc2nc3ccccc3n2-c2cccc3cccnc23)CC1>[Pd].CO>CC(C)C(=O)CN1CCC(Nc2nc3ccccc3n2-c2cccc3c2NCCC3)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-777e8d975bae46508dbc8e95dcfff963
N#CCCl.c1ccc2c(Cn3c(NC4CCNCC4)nc4ccccc43)ccnc2c1>>N#CCN1CCC(Nc2nc3ccccc3n2Cc2ccnc3ccccc23)CC1
N1CCC(CC1)NC1=NC2=C(N1CC1=CC=NC3=CC=CC=C13)C=CC=C2.ClCC#N.[I-].[K+].C([O-])([O-])=O.[K+].[K+]>>N1=CC=C(C2=CC=CC=C12)CN1C(=NC2=C1C=CC=C2)NC2CCN(CC2)CC#N
Cl[CH2:3][C:2]#[N:1].[NH:4]1[CH2:5][CH2:6][CH:7]([NH:8][c:9]2[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[n:17]2[CH2:18][c:19]2[cH:20][cH:21][n:22][c:23]3[cH:24][cH:25][cH:26][cH:27][c:28]23)[CH2:29][CH2:30]1>>[N:1]#[C:2][CH2:3][N:4]1[CH2:5][CH2:6][CH:7]([NH:8][c:9]2[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[...
N#CCCl.c1ccc2c(Cn3c(NC4CCNCC4)nc4ccccc43)ccnc2c1
N#CCN1CCC(Nc2nc3ccccc3n2Cc2ccnc3ccccc23)CC1
null
null
O.CC(CC(C)=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc2c(Cn3c(NC4CCNCC4)nc4ccccc43)ccnc2c1
Cl-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3].[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]#[N;D1;H0:3])-[C:7]-[C:8]
18.4
[{"value": 18.4, "product": "N1=CC=C(C2=CC=CC=C12)CN1C(=NC2=C1C=CC=C2)NC2CCN(CC2)CC#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of N-(4-piperidinyl)-1-(4-quinolinylmethyl)-1H-benzimidazol-2-amine (comp. 23) (0.0129 mol), chloroacetonitrile (0.0155 mol), potassium iodide (0.00129 mol) and potassium carbonate (0.0258 mol) in 4-methyl-2-pentanone (80 ml) was stirred and refluxed for 5 hours. H2O was added. The solvent was evaporated. H2O...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1nc2ccccc2[nH]1.c1ccc2ncccc2c1
HCl
O.CC(CC(C)=O)C
null
null
N#CCCl.c1ccc2c(Cn3c(NC4CCNCC4)nc4ccccc43)ccnc2c1>O.CC(CC(C)=O)C>N#CCN1CCC(Nc2nc3ccccc3n2Cc2ccnc3ccccc23)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0087de8c0dd14e0d8ed5fc816b51a058
CC#N.CCOC(c1nc2ccccc2cc1OC)n1c(NC2CCNCC2)nc2ccccc21.O=C([O-])[O-]>>CCOC(c1nc2ccccc2cc1OC)n1c(NC2CCN(CC(NC(=O)OC(C)(C)C)C(C)C)CC2)nc2ccccc21
C(C)OC(N1C(=NC2=C1C=CC=C2)NC2CCNCC2)C2=NC1=CC=CC=C1C=C2OC.C([O-])([O-])=O.[K+].[K+].C(C)#N>>C(C)OC(N1C(=NC2=C1C=CC=C2)NC2CCN(CC2)CC(C(C)C)NC(OC(C)(C)C)=O)C2=NC1=CC=CC=C1C=C2OC
[CH3:24][C:25]#[N:26].[CH3:1][CH2:2][O:3][CH:4]([c:5]1[n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[cH:13][c:14]1[O:15][CH3:16])[n:17]1[c:18]([NH:19][CH:20]2[CH2:21][CH2:22][NH:23][CH2:37][CH2:38]2)[n:39][c:40]2[cH:41][cH:42][cH:43][cH:44][c:45]12.[O-][C:27](=[O:28])[O-:29]>>[CH3:1][CH2:2][O:3][CH:4]([c:5]1[n:6][c:7]2[c...
CC#N.CCOC(c1nc2ccccc2cc1OC)n1c(NC2CCNCC2)nc2ccccc21.O=C([O-])[O-]
CCOC(c1nc2ccccc2cc1OC)n1c(NC2CCN(CC(NC(=O)OC(C)(C)C)C(C)C)CC2)nc2ccccc21
null
null
CN(C)C=O
C-C Coupling
OtherReaction
86b124de698592091f05727e0d9cafd3b33acc7cb0420d7cca188b435c895043
937da2521b5452a60917b079f45a86f63903cfd1df228982b69ca749b25f83f7
c1ccc2nc(Cn3c(NC4CCNCC4)nc4ccccc43)ccc2c1
[CH3;D1;+0:1]-[C;H0;D2;+0:2]#[N;H0;D1;+0:3].[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8].[O-;H0;D1:9]-[C;H0;D3;+0:10](-[O-])=[O;D1;H0:11]>>[C:4]-[C:5]-[N;H0;D3;+0:6](-[CH2;D2;+0:1]-[CH;D3;+0:2](-[NH;D2;+0:3]-[C;H0;D3;+0:10](=[O;D1;H0:11])-[O;H0;D2;+0:9]-[C:12](-[C;D1;H3:13])(-[C;D1;H3:14])-[C;D1;H3:15])-[C:16](-[C;D1;H3:17])-[...
23
[{"value": 23.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
55
CELSIUS
1
HOUR
Intermediate (32) (0.1382 mol) was added at 55° C. to a mixture of (±)-1-[ethoxy(3-methoxy-2-quinolinyl)methyl]-N-(4-piperidinyl)-1H-benzimidazol-2-amine (0.0346 mol) and potassium carbonate (0.242 mol) in acetonitrile (108 ml) and DMF (20 ml) (1 equiv of intermediate (32) was added every hour). The mixture was stirred...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Secondary amine
Carbamic ester.Ether.Tertiary amine.Boc
C1CCNCC1
C1CC[NH]CC1
c1ccc2ncccc2c1.C1CC[NH]CC1.c1nc2ccccc2[nH]1
null
CN(C)C=O
55
1
CC#N.CCOC(c1nc2ccccc2cc1OC)n1c(NC2CCNCC2)nc2ccccc21.O=C([O-])[O-]>CN(C)C=O>CCOC(c1nc2ccccc2cc1OC)n1c(NC2CCN(CC(NC(=O)OC(C)(C)C)C(C)C)CC2)nc2ccccc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5cbaa8d5463e48db9ab3b9ad615b1d9a
COc1cc2c(nc1Cn1c(NC3CCN(CC(N)C(C)C)CC3)nc3ccccc31)CCCC2.Cl.Cl>>CC(C)C(N)CN1CCC(Nc2nc3ccccc3n2Cc2nc3c(cc2O)CCCC3)CC1.Cl.Cl
[NH4+].[OH-].O.Cl.Cl.Cl.Cl.NC(CN1CCC(CC1)NC1=NC2=C(N1CC1=NC=3CCCCC3C=C1OC)C=CC=C2)C(C)C.C(=O)([O-])[O-].[K+].[K+].BrB(Br)Br>>O.Cl.Cl.Cl.Cl.NC(CN1CCC(CC1)NC1=NC2=C(N1CC1=NC=3CCCCC3C=C1O)C=CC=C2)C(C)C
C[O:28][c:27]1[c:22]([CH2:21][n:20]2[c:12]([NH:11][CH:10]3[CH2:9][CH2:8][N:7]([CH2:6][CH:4]([CH:2]([CH3:1])[CH3:3])[NH2:5])[CH2:34][CH2:33]3)[n:13][c:14]3[cH:15][cH:16][cH:17][cH:18][c:19]32)[n:23][c:24]2[c:25]([cH:26]1)[CH2:32][CH2:31][CH2:30][CH2:29]2.[ClH:36].[ClH:38]>>[CH3:1][CH:2]([CH3:3])[CH:4]([NH2:5])[CH2:6][N:...
COc1cc2c(nc1Cn1c(NC3CCN(CC(N)C(C)C)CC3)nc3ccccc31)CCCC2.Cl.Cl
CC(C)C(N)CN1CCC(Nc2nc3ccccc3n2Cc2nc3c(cc2O)CCCC3)CC1.Cl.Cl
null
null
ClCCl
C-C Coupling
OtherReaction
5041c0a04bc37f2e4389098854967a21b078c8276fd88e518dbe1383c1b59387
7e7da33d0069dcc5669156a71f2ea38e16dcea58a7086356ac070b4210cbe68b
c1ccc2c(c1)nc(NC1CCNCC1)n2Cc1ccc2c(n1)CCCC2
C-[O;H0;D2;+0:1]-[c:2]1:[c:3]:[c;H0;D3;+0:4]2:[c;H0;D3;+0:5](:[#7;a:6]:[c:7]:1-[C:8])-[CH2;D2;+0:9]-[C:10]-[C:11]-[CH2;D2;+0:12]-2>>[C:8]-[c:7]1:[#7;a:6]:[c;H0;D3;+0:5]2:[c;H0;D3;+0:4](:[c:3]:[c:2]:1-[OH;D1;+0:1])-[CH2;D2;+0:9]-[C:10]-[C:11]-[CH2;D2;+0:12]-2
37
[{"value": 37.0, "product": "O.Cl.Cl.Cl.Cl.NC(CN1CCC(CC1)NC1=NC2=C(N1CC1=NC=3CCCCC3C=C1O)C=CC=C2)C(C)C", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
8
HOUR
(±)-N-[1-(2-amino-3-methylbutyl)-4-piperidinyl]-1-[(5,6,7,8-tetrahydro-3-methoxy-2-quinolinyl)methyl]-1H-benzimidazol-2-amine tetrahydrochloride monohydrate (0.0021—O— mol) was basified with K2CO3 10%. The mixture was extracted with CH2Cl2. The organic layer was separated, dried (MgSO4), filtered and the solvent was ev...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
c1cnc2c(c1)CCCC2
c1cnc2c(c1)CCCC2
C1CC[NH]CC1.c1nc2ccccc2[nH]1.c1cnc2c(c1)CCCC2
Other
ClCCl
0
8
COc1cc2c(nc1Cn1c(NC3CCN(CC(N)C(C)C)CC3)nc3ccccc31)CCCC2.Cl.Cl>ClCCl>CC(C)C(N)CN1CCC(Nc2nc3ccccc3n2Cc2nc3c(cc2O)CCCC3)CC1.Cl.Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bb490914043a4089a4b4985a7be43596
C1CCNCC1.O=Cc1ccc(O)cc1>>Oc1ccc(CN2CCCCC2)cc1
C([O-])(O)=O.[Na+].OC1=CC=C(C=O)C=C1.N1CCCCC1.C(C)(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+]>>N1(CCCCC1)CC1=CC=C(C=C1)O
[NH:7]1[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1.O=[CH:6][c:5]1[cH:4][cH:3][c:2]([OH:1])[cH:14][cH:13]1>>[OH:1][c:2]1[cH:3][cH:4][c:5]([CH2:6][N:7]2[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)[cH:13][cH:14]1
C1CCNCC1.O=Cc1ccc(O)cc1
Oc1ccc(CN2CCCCC2)cc1
null
null
C(C)(=O)O.ClCCCl
Heteroatom Alkylation and Arylation
reductive amination
d0e659bc8d1e29e09a61320b4c537e66ad57335a51368c8bd48de9bdffa59372
2d03f38884b1fbb0c0d6e6f2de31afb25102fec87f347c3a123e064c1bfef0ad
c1ccc(CN2CCCCC2)cc1
O=[CH;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]
null
[]
null
null
16
HOUR
A solution of 4-hydroxybenzaldehyde (10 g), piperidine (8.9 mL), and acetic acid (4.7 mL) in DCE (200 mL) was treated with sodium triacetoxyborohydride (24 g). After 16 h, the resulting mixture was treated with saturated aqueous sodium bicarbonate (100 mL) and extracted with DCM (5×100 mL). The combined organic phases ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1
Other
C(C)(=O)O.ClCCCl
null
16
C1CCNCC1.O=Cc1ccc(O)cc1>C(C)(=O)O.ClCCCl>Oc1ccc(CN2CCCCC2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-346124e808e24aa7ad3300eb46a48213
CC(C)(C)OC(=O)N1CCC(O)CC1.CC(C)(C)OC(=O)N1CCN(c2ccc(O)cc2)CC1>>CC(C)(C)OC(=O)N1CCC(Oc2ccc(N3CCN(C(=O)OC(C)(C)C)CC3)cc2)CC1
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(C)(C)(C)OC(=O)N1CCN(CC1)C1=CC=C(C=C1)O.C(C)(C)(C)OC(=O)N1CCC(CC1)O.CC(C)(C)OC(=O)/N=N/C(=O)OC(C)(C)C>>C(C)(C)(C)OC(=O)N1CCN(CC1)C1=CC=C(C=C1)OC1CCN(CC1)C(=O)OC(C)(C)C
O[CH:11]1[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:33][CH2:32]1.[OH:12][c:13]1[cH:14][cH:15][c:16]([N:17]2[CH2:18][CH2:19][N:20]([C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27])[CH2:28][CH2:29]2)[cH:30][cH:31]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:1...
CC(C)(C)OC(=O)N1CCC(O)CC1.CC(C)(C)OC(=O)N1CCN(c2ccc(O)cc2)CC1
CC(C)(C)OC(=O)N1CCC(Oc2ccc(N3CCN(C(=O)OC(C)(C)C)CC3)cc2)CC1
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether
a9e936b0e9135225700edbab1c7696738b7f1f0756494b6ceeeda63b184d572f
776ba735002e33225fbc578943016110c2c43efefd97bfeea4ec3cc2e2e1532f
c1cc(N2CCNCC2)ccc1OC1CCNCC1
O-[CH;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1.[OH;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[c:9]:[c:8](-[O;H0;D2;+0:7]-[CH;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1):[c:10]
62
[{"value": 15.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.0, "product": "C(C)(C)(C)OC(=O)N1CCN(CC1)C1=CC=C(C=C1)OC1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A suspension of 4-(4-Hydroxy-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (3.11 g), 4-Hydroxy-piperidine-1-carboxylic acid tert-butyl ester (3.51 g), and polymer supported triphenylphosphine (6.25 g; loading: 3 mmol/g) in DCM (100 mL) was treated with di-tert-butylazodicarboxylate (3.78 g). After 24 h, the res...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Aromatic alcohol
Ether
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccccc1.C1C[NH]CC[NH]1
HO-
C(Cl)Cl
null
24
CC(C)(C)OC(=O)N1CCC(O)CC1.CC(C)(C)OC(=O)N1CCN(c2ccc(O)cc2)CC1>C(Cl)Cl>CC(C)(C)OC(=O)N1CCC(Oc2ccc(N3CCN(C(=O)OC(C)(C)C)CC3)cc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e3fc973aa2db4d2bb873ff11623b4a2f
CCC[CH2][Sn]([Cl])([Cl])[CH2]CCC.c1cn(-c2ccc(OC3CCNCC3)cc2)cn1>>CC(C)CN1CCC(Oc2ccc(-n3ccnc3)cc2)CC1
N1(C=NC=C1)C1=CC=C(OC2CCNCC2)C=C1.C1(CCCCC1)=O.C(CCC)[Sn](CCCC)(Cl)Cl.C1(=CC=CC=C1)[SiH3]>>N1(C=NC=C1)C1=CC=C(OC2CCN(CC2)CC(C)C)C=C1
C[CH2:3][CH2:2][CH2:4][Sn]([Cl])([Cl])[CH2]CC[CH3:1].[NH:5]1[CH2:6][CH2:7][CH:8]([O:9][c:10]2[cH:11][cH:12][c:13](-[n:14]3[cH:15][cH:16][n:17][cH:18]3)[cH:19][cH:20]2)[CH2:21][CH2:22]1>>[CH3:1][CH:2]([CH3:3])[CH2:4][N:5]1[CH2:6][CH2:7][CH:8]([O:9][c:10]2[cH:11][cH:12][c:13](-[n:14]3[cH:15][cH:16][n:17][cH:18]3)[cH:19][...
CCC[CH2][Sn]([Cl])([Cl])[CH2]CCC.c1cn(-c2ccc(OC3CCNCC3)cc2)cn1
CC(C)CN1CCC(Oc2ccc(-n3ccnc3)cc2)CC1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
c5453a8b22dde1752bbee9d938fa6c1b29b157df3ee3efeb36640e89adbe6533
92c4050b7b70356e79fb7d199a0bcda4cb4fb71f721dd8f555006485a88111eb
c1cn(-c2ccc(OC3CCNCC3)cc2)cn1
C-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[CH2;D2;+0:3]-[Sn](-[Cl])(-[Cl])-[CH2]-C-C-[CH3;D1;+0:4].[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]>>[C:5]-[C:6]-[N;H0;D3;+0:7](-[CH2;D2;+0:3]-[CH;D3;+0:2](-[CH3;D1;+0:4])-[CH3;D1;+0:1])-[C:8]-[C:9]
null
[]
null
null
16
HOUR
A solution of the product of Example 6 (130 mg), cyclohexanone (0.06 mL), and dibutyltin dichloride (3 mg) in THF (0.1 mL) was treated with phenylsilane (0.07 mL). After 16 h, the resulting mixture was chromatographed (0-8% 2M methanolic ammonia/DCM), giving the title compound as a waxy solid (18 mg). 1H NMR (400 MHz, ...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Tin
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccccc1.c1c[nH]cn1
HCl.Sn
C1CCOC1
null
16
CCC[CH2][Sn]([Cl])([Cl])[CH2]CCC.c1cn(-c2ccc(OC3CCNCC3)cc2)cn1>C1CCOC1>CC(C)CN1CCC(Oc2ccc(-n3ccnc3)cc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8fad9727d68f44a9901ab1ec5c51fcfb
CC(C)C=O.CCC[CH2][Sn]([Cl])([Cl])[CH2]CCC.c1cn(-c2ccc(OC3CCNCC3)cc2)cn1>>c1cn(-c2ccc(OC3CCN(C4CCCC4)CC3)cc2)cn1
N1(C=NC=C1)C1=CC=C(OC2CCNCC2)C=C1.C(C(C)C)=O.C(CCC)[Sn](CCCC)(Cl)Cl.C1(=CC=CC=C1)[SiH3]>>C1(CCCC1)N1CCC(CC1)OC1=CC=C(C=C1)N1C=NC=C1
C[CH:17]([CH:13]=O)[CH3:14].CCC[CH2][Sn]([Cl])([Cl])[CH2]C[CH2:16][CH3:15].[cH:1]1[cH:2][n:3](-[c:4]2[cH:5][cH:6][c:7]([O:8][CH:9]3[CH2:10][CH2:11][NH:12][CH2:18][CH2:19]3)[cH:20][cH:21]2)[cH:22][n:23]1>>[cH:1]1[cH:2][n:3](-[c:4]2[cH:5][cH:6][c:7]([O:8][CH:9]3[CH2:10][CH2:11][N:12]([CH:13]4[CH2:14][CH2:15][CH2:16][CH2:...
CC(C)C=O.CCC[CH2][Sn]([Cl])([Cl])[CH2]CCC.c1cn(-c2ccc(OC3CCNCC3)cc2)cn1
c1cn(-c2ccc(OC3CCN(C4CCCC4)CC3)cc2)cn1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
3e5326fa41f36adea6aacee576b720dc36b92c0952de7bdf859daff8cbf3d9a4
2aaed6d073b4fd8753dfdb27d6b51aa16006392671408dbe672ad3d6f8fa14f6
c1cn(-c2ccc(OC3CCN(C4CCCC4)CC3)cc2)cn1
C-C-C-[CH2]-[Sn](-[Cl])(-[Cl])-[CH2]-C-[CH2;D2;+0:1]-[CH3;D1;+0:2].C-[CH;D3;+0:3](-[CH3;D1;+0:4])-[CH;D2;+0:5]=O.[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[CH;D3;+0:5]1-[CH2;D2;+0:4]-[CH2;D2;+0:2]-[CH2;D2;+0:1]-[CH2;D2;+0:3]-1)-[C:9]-[C:10]
null
[]
null
null
16
HOUR
A solution of the product of Example 6 (130 mg), isobutyraldehyde (0.06 mL), and dibutyltin dichloride (3 mg) in THF (0.1 mL) was treated with phenylsilane (0.07 mL). After 16 h, the resulting mixture was chromatographed (0-8% 2M methanolic ammonia/DCM), giving the title compound as a waxy solid (57 mg). 1H NMR (400 MH...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine.Tin
Tertiary amine
C1CCNCC1
C1CC[NH]CC1.C1CCCC1
c1c[nH]cn1.c1ccccc1.C1CC[NH]CC1.C1CCCC1
HCl.Sn
C1CCOC1
null
16
CC(C)C=O.CCC[CH2][Sn]([Cl])([Cl])[CH2]CCC.c1cn(-c2ccc(OC3CCNCC3)cc2)cn1>C1CCOC1>c1cn(-c2ccc(OC3CCN(C4CCCC4)CC3)cc2)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cc38c2af609146af82a40efe6716b1ba
CC(C)(C)OC(=O)N1CCC(O)CC1.CC(C)(C)OC(=O)N=NC(=O)OC(C)(C)C.Oc1ccc(-c2ccccc2)cc1>>N.c1ccc(-c2ccc(OC3CCNCC3)cc2)cc1
OC1CCN(CC1)C(=O)OC(C)(C)C.C1(=CC=CC=C1)C1=CC=C(C=C1)O.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(Cl)Cl.N(=NC(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>N.C(Cl)Cl.C1(=CC=C(C=C1)OC1CCNCC1)C1=CC=CC=C1
CC(C)(C)OC(=O)[N:17]1[CH2:16][CH2:15][CH:14]([OH:13])[CH2:19][CH2:18]1.CC(C)(C)OC(=O)N=[N:4]C(=O)OC(C)(C)C.O[c:12]1[cH:11][cH:10][c:9](-[c:8]2[cH:7][cH:6][cH:5][cH:23][cH:22]2)[cH:21][cH:20]1>>[NH3:4].[cH:5]1[cH:6][cH:7][c:8](-[c:9]2[cH:10][cH:11][c:12]([O:13][CH:14]3[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]3)[cH:20][cH:...
CC(C)(C)OC(=O)N1CCC(O)CC1.CC(C)(C)OC(=O)N=NC(=O)OC(C)(C)C.Oc1ccc(-c2ccccc2)cc1
N.c1ccc(-c2ccc(OC3CCNCC3)cc2)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
fe7e504d552b31842d25f2c9c0e3e359bfac598abef74c57c464b9a7d9eef99d
fffd8854affd038b0da6a0ed69aea71c9302d200efe0a706572ca9c6fcfe89ad
c1ccc(-c2ccc(OC3CCNCC3)cc2)cc1
C-C(-C)(-C)-O-C(=O)-N=[N;H0;D2;+0:1]-C(=O)-O-C(-C)(-C)-C.C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:2]1-[C:3]-[C:4]-[C:5](-[OH;D1;+0:6])-[C:7]-[C:8]-1.O-[c;H0;D3;+0:9](:[c:10]:[c:11]):[c:12]:[c:13]>>[NH3;D0;+0:1].[c:11]:[c:10]:[c;H0;D3;+0:9](-[O;H0;D2;+0:6]-[C:5]1-[C:4]-[C:3]-[NH;D2;+0:2]-[C:8]-[C:7]-1):[c:12]:[c:13]
1
[{"value": 1.0, "product": "N.C(Cl)Cl", "details": "PERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
A suspension of tert-butyl 4-hydroxy-1-piperidine carboxylate (497 mg), 4-phenylphenol (300 mg), and polymer-supported triphenylphosphine (1.2 g) in DCM (10 mL) was treated with di-tert-butyl azodicarboxylate (608 mg). The resulting mixture was shaken for 16 h, and filtered through a pad of celite. The pad was washed w...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Diazene.Secondary alcohol.Aromatic alcohol.Boc.Boc.Boc
Ether.Secondary amine
C1CC[NH]CC1.c1ccccc1
c1ccccc1.C1CCNCC1
c1ccccc1.c1ccccc1.C1CCNCC1
HO-
null
null
16
CC(C)(C)OC(=O)N1CCC(O)CC1.CC(C)(C)OC(=O)N=NC(=O)OC(C)(C)C.Oc1ccc(-c2ccccc2)cc1>>N.c1ccc(-c2ccc(OC3CCNCC3)cc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a7df8718c86049db81c9d8953d000404
CCOC=O.N#CCC1CCCC1>>N#CC(C=O)C1CCCC1
C1(CCCC1)CC#N.CCCCC.C(=O)OCC>>C1(CCCC1)C(C=O)C#N
CCO[CH:4]=[O:5].[N:1]#[C:2][CH2:3][CH:6]1[CH2:7][CH2:8][CH2:9][CH2:10]1>>[N:1]#[C:2][CH:3]([CH:4]=[O:5])[CH:6]1[CH2:7][CH2:8][CH2:9][CH2:10]1
CCOC=O.N#CCC1CCCC1
N#CC(C=O)C1CCCC1
null
null
O1CCCC1
C-C Coupling
OtherReaction
3dc7150b54f968d08b04811ce6d9fd58ce6b1717b4fbd76dbd02e91654c50b43
2aa39a25981921b5291a5742361ce4441cd47a0f2b930c869f26329c906b19c5
C1CCCC1
C-C-O-[CH;D2;+0:1]=[O;D1;H0:2].[C:3]-[C:4](-[CH2;D2;+0:5]-[C:6]#[N;D1;H0:7])-[C:8]>>[C:3]-[C:4](-[CH;D3;+0:5](-[C:6]#[N;D1;H0:7])-[CH;D2;+0:1]=[O;D1;H0:2])-[C:8]
null
[]
-60
CELSIUS
10
MINUTE
A mixture of 2-cyclopentylacetonitrile (0.50 g, 4.59 mmol) in tetrahydrofuran (10 mL) was cooled to −60° C. then treated with 1.7 M tert-buytllithium in pentane (3.25 mL, 5.50 mmol) while maintaining the reaction temperature at less than −55° C. The solution was stirred for 10 minutes then ethyl formate (0.41 g, 5.50 m...
10.6084/m9.figshare.5104873.v1
null
Ether
Aldehyde
null
null
C1CCCC1
HO-
O1CCCC1
-60
0.166667
CCOC=O.N#CCC1CCCC1>O1CCCC1>N#CC(C=O)C1CCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9a2b2b67968740b09716865dce6a705d
N#CCBr.Nc1ccc(Oc2ccccc2)cc1>>N#CCNc1ccc(Oc2ccccc2)cc1
BrCC#N.O(C1=CC=CC=C1)C1=CC=C(N)C=C1.BrCC#N.C(C)N(CC)CC>>O(C1=CC=CC=C1)C1=CC=C(NCC#N)C=C1
Br[CH2:3][C:2]#[N:1].[NH2:4][c:5]1[cH:6][cH:7][c:8]([O:9][c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)[cH:16][cH:17]1>>[N:1]#[C:2][CH2:3][NH:4][c:5]1[cH:6][cH:7][c:8]([O:9][c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)[cH:16][cH:17]1
N#CCBr.Nc1ccc(Oc2ccccc2)cc1
N#CCNc1ccc(Oc2ccccc2)cc1
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
fc19a1445ff204e66e51735d0191465bda3c6691fd233624a54742c9d4828411
0b1d32f56ad00f1e5bdae9390f9227bbea012fa2f8203aac34726b8a6761cc7c
c1ccc(Oc2ccccc2)cc1
Br-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[N;D1;H0:3]#[C:2]-[CH2;D2;+0:1]-[NH;D2;+0:4]-[c:5](:[c:6]):[c:7]
45
[{"value": 45.0, "product": "O(C1=CC=CC=C1)C1=CC=C(NCC#N)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 44.8, "product": "O(C1=CC=CC=C1)C1=CC=C(NCC#N)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
A mixture of 4-phenoxyaniline (7.0 g, 37.8 mmol), bromoacetonitrile (4.5 g, 37.8 mmol) and triethylamine (4.2 g, 41.6 mmol) in tetrahydrofuran (50 mL) was heated at 85° C. for 5.25 hours then cooled and another portion of bromoacetonitrile (6.5 g, 5.46 mmol) was added. The mixture was heated at 85° C. for 18 hours then...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary amine
Secondary amine
null
null
c1ccccc1.c1ccccc1
HBr
O1CCCC1
85
null
N#CCBr.Nc1ccc(Oc2ccccc2)cc1>O1CCCC1>N#CCNc1ccc(Oc2ccccc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7a119e6b380e48b1928402a388d28815
N#Cc1c(N)c(C2CCCC2)cn1-c1ccc(Oc2ccccc2)cc1.N=CN>>Nc1ncnc2c(C3CCCC3)cn(-c3ccc(Oc4ccccc4)cc3)c12
NC1=C(N(C=C1C1CCCC1)C1=CC=C(C=C1)OC1=CC=CC=C1)C#N.C(C)(=O)O.C(=N)N>>C1(CCCC1)C1=CN(C2=C1N=CN=C2N)C2=CC=C(C=C2)OC2=CC=CC=C2
[N:1]#[C:2][c:28]1[c:6]([NH2:5])[c:7]([CH:8]2[CH2:9][CH2:10][CH2:11][CH2:12]2)[cH:13][n:14]1-[c:15]1[cH:16][cH:17][c:18]([O:19][c:20]2[cH:21][cH:22][cH:23][cH:24][cH:25]2)[cH:26][cH:27]1.N[CH:4]=[NH:3]>>[NH2:1][c:2]1[n:3][cH:4][n:5][c:6]2[c:7]([CH:8]3[CH2:9][CH2:10][CH2:11][CH2:12]3)[cH:13][n:14](-[c:15]3[cH:16][cH:17]...
N#Cc1c(N)c(C2CCCC2)cn1-c1ccc(Oc2ccccc2)cc1.N=CN
Nc1ncnc2c(C3CCCC3)cn(-c3ccc(Oc4ccccc4)cc3)c12
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
f19dbf5d03a6825dd5f8c304f8d6f3418a6ebdaf9f0b55bd20edc2f3f8ce34be
1aa7191beb21c0c960b18631a0bd52edc8e0a5e54fb7edd4fc42913ae18d9901
c1ccc(Oc2ccc(-n3cc(C4CCCC4)c4ncncc43)cc2)cc1
N-[CH;D2;+0:1]=[NH;D1;+0:2].[N;H0;D1;+0:3]#[C;H0;D2;+0:4]-[c:5]1:[#7;a:6](-[c:7]):[c:8]:[c:9]:[c:10]:1-[NH2;D1;+0:11]>>[NH2;D1;+0:3]-[c;H0;D3;+0:4]1:[n;H0;D2;+0:2]:[cH;D2;+0:1]:[n;H0;D2;+0:11]:[c:10]2:[c:9]:[c:8]:[#7;a:6](-[c:7]):[c:5]:2:1
73
[{"value": 73.0, "product": "C1(CCCC1)C1=CN(C2=C1N=CN=C2N)C2=CC=C(C=C2)OC2=CC=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.6, "product": "C1(CCCC1)C1=CN(C2=C1N=CN=C2N)C2=CC=C(C=C2)OC2=CC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
A mixture of the 3-amino-4-cyclopentyl-1-(4-phenoxyphenyl)-1H-2-pyrrolecarbonitrile (185 mg, 0.539 mmol) in absolute ethanol (10 mL) was treated with formamidine acetate (450 mg, 4.33 mmol) then heated at 85° C. for 2 hours. The solvent was evaporated under reduced pressure then the residue was purified by preparative ...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Primary amine.Primary amine
Primary amine
c1cc[nH]c1
c1c[nH]c2cncnc12
C1CCCC1.c1c[nH]c2cncnc12.c1ccccc1.c1ccccc1
Other
C(C)O
85
null
N#Cc1c(N)c(C2CCCC2)cn1-c1ccc(Oc2ccccc2)cc1.N=CN>C(C)O>Nc1ncnc2c(C3CCCC3)cn(-c3ccc(Oc4ccccc4)cc3)c12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3ea04bd552ac4d0fbd04f91758f9a726
N#Cc1ccn(C2CCCC2)c1C=O.NN>>Nc1nncc2c1ccn2C1CCCC1
C1(CCCC1)N1C(=C(C=C1)C#N)C=O.Cl.Cl.NN>>C1(CCCC1)N1C=CC=2C1=CN=NC2N
O=[CH:5][c:6]1[c:7]([C:2]#[N:1])[cH:8][cH:9][n:10]1[CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15]1.[NH2:3][NH2:4]>>[NH2:1][c:2]1[n:3][n:4][cH:5][c:6]2[c:7]1[cH:8][cH:9][n:10]2[CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15]1
N#Cc1ccn(C2CCCC2)c1C=O.NN
Nc1nncc2c1ccn2C1CCCC1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
377eac503eaf096d8edd56661268db2947dc5624a15c5ab2472e3e0e61e27ee4
fa59c52dd5da416f757f65367be99eabbf642b5454b61e6f56bbb37a09927483
c1cn(C2CCCC2)c2cnncc12
O=[CH;D2;+0:1]-[c:2]1:[#7;a:3](-[C:4]):[c:5]:[c:6]:[c:7]:1-[C;H0;D2;+0:8]#[N;H0;D1;+0:9].[NH2;D1;+0:10]-[NH2;D1;+0:11]>>[C:4]-[#7;a:3]1:[c:5]:[c:6]:[c:7]2:[c:2]:1:[cH;D2;+0:1]:[n;H0;D2;+0:11]:[n;H0;D2;+0:10]:[c;H0;D3;+0:8]:2-[NH2;D1;+0:9]
null
[]
null
null
null
null
A mixture of 1-cyclopentyl-2-formyl-1H-3-pyrrolecarbonitrile (0.525 g, 2.79 mmol) and hydrazine dihydrochloride (0.35 g, 3.35 mmol) in ethanol (30 mL) was heated at reflux for 2.5 hours then cooled to ambient temperature and purified by preparative reverse phase HPLC to give the title compound as a hydroscopic glass co...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Aldehyde.Nitrile
Primary amine
c1c[nH]cc1
c1nncc2[nH]ccc12
c1nncc2[nH]ccc12.C1CCCC1
HO-
C(C)O
null
null
N#Cc1ccn(C2CCCC2)c1C=O.NN>C(C)O>Nc1nncc2c1ccn2C1CCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a4b076179dca456485413d3e1e416279
BrBr.Nc1nncc2c1ccn2C1CCCC1>>Nc1nncc2c1c(Br)cn2C1CCCC1
BrBr.C1(CCCC1)N1C=CC=2C1=CN=NC2N.BrBr.[OH-].[Na+].O>>BrC1=CN(C2=CN=NC(=C21)N)C2CCCC2
Br[Br:9].[NH2:1][c:2]1[n:3][n:4][cH:5][c:6]2[c:7]1[cH:8][cH:10][n:11]2[CH:12]1[CH2:13][CH2:14][CH2:15][CH2:16]1>>[NH2:1][c:2]1[n:3][n:4][cH:5][c:6]2[c:7]1[c:8]([Br:9])[cH:10][n:11]2[CH:12]1[CH2:13][CH2:14][CH2:15][CH2:16]1
BrBr.Nc1nncc2c1ccn2C1CCCC1
Nc1nncc2c1c(Br)cn2C1CCCC1
null
null
ClCCl
Functional Group Interconversion
Bromination
e8a70d132c5b93ca409b6111f13d0cba041e6984c4f07d40dc0d4a3acc6a74ba
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1cn(C2CCCC2)c2cnncc12
Br-[Br;H0;D1;+0:1].[C:2]-[#7;a:3]1:[c:4]:[cH;D2;+0:5]:[c:6]2:[c:7](-[N;D1;H2:8]):[#7;a:9]:[#7;a:10]:[c:11]:[c:12]:1:2>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:5]1:[c:4]:[#7;a:3](-[C:2]):[c:12]2:[c:11]:[#7;a:10]:[#7;a:9]:[c:7](-[N;D1;H2:8]):[c:6]:2:1
35
[{"value": 35.0, "product": "BrC1=CN(C2=CN=NC(=C21)N)C2CCCC2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 34.0, "product": "BrC1=CN(C2=CN=NC(=C21)N)C2CCCC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A mixture of 1-cyclopentyl-1H-pyrrolo[2,3-d]pyridazin-4-amine (0.595 mg, approx. 60% pure, 1.76 mmol) in dichloromethane (100 mL) was treated with a solution of dichloromethane (5 mL) containing bromine (0.5 g, 2.95 mmol) over the course of 1.25 hours. The mixture was stirred an additional one hour then another portion...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1nncc2[nH]ccc12
c1c[nH]c2cnncc12
c1c[nH]c2cnncc12.C1CCCC1
HBr
ClCCl
null
1
BrBr.Nc1nncc2c1ccn2C1CCCC1>ClCCl>Nc1nncc2c1c(Br)cn2C1CCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4ee0e95287a3428ba9b400d4a0569d2f
Nc1nncc2c1c(Br)cn2C1CCCC1>>Nc1nncc2c1c(-c1ccc(Oc3ccccc3)cc1)cn2C1CCCC1
BrC1=CN(C2=CN=NC(=C21)N)C2CCCC2.O(C1=CC=CC=C1)C1=CC=C(C=C1)B(O)O.C([O-])([O-])=O.[Na+].[Na+]>>C1(CCCC1)N1C=C(C=2C1=CN=NC2N)C2=CC=C(C=C2)OC2=CC=CC=C2.O(C1=CC=CC=C1)C1=CC=C(C=C1)B(O)O
Br[c:8]1[c:7]2[c:2]([NH2:1])[n:3][n:4][cH:5][c:6]2[n:23]([CH:24]2[CH2:25][CH2:26][CH2:9][CH2:28]2)[cH:22]1>>[NH2:1][c:2]1[n:3][n:4][cH:5][c:6]2[c:7]1[c:8](-[c:9]1[cH:10][cH:11][c:12]([O:13][c:14]3[cH:15][cH:16][cH:17][cH:18][cH:19]3)[cH:20][cH:21]1)[cH:22][n:23]2[CH:24]1[CH2:25][CH2:26][CH2:27][CH2:28]1
Nc1nncc2c1c(Br)cn2C1CCCC1
Nc1nncc2c1c(-c1ccc(Oc3ccccc3)cc1)cn2C1CCCC1
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
O.COCCOC
Aromatic Heterocycle Formation
OtherReaction
f27a42616b1c67cdcd393f1a4700264031759bc4e8cecd2cb09f5db1c966dbe3
a4840aa8bdfd6f728c7dfa6c00c462c0316cfea6c6529f068981467c19c289cb
c1ccc(Oc2ccc(-c3cn(C4CCCC4)c4cnncc34)cc2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3](-[C:4]2-[C:5]-[CH2;D2;+0:6]-[CH2;D2;+0:7]-[CH2;D2;+0:8]-2):[c:9]2:[c:10]:[#7;a:11]:[#7;a:12]:[c:13](-[N;D1;H2:14]):[c:15]:2:1>>[N;D1;H2:14]-[c:13]1:[#7;a:12]:[#7;a:11]:[c:10]:[c:9]2:[#7;a:3](-[C:4]3-[C:5]-[CH2;D2;+0:6]-[C:16]-[CH2;D2;+0:8]-3):[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:7](:[c:17...
null
[]
85
CELSIUS
null
null
A mixture of 3-bromo-1-cyclopentyl-1H-pyrrolo [2,3-d]pyridazin-4-amine (0.057 g, 0.178 mmol), 4-phenoxyphenyl boronic acid (0.057 g, 0.266 mmol), sodium carbonate (0.062 g, 0.588 mmol) and tetrakis(triphenylphosphine)palladium(0) (12 mg, 0.011 mmol) in ethylene glycol dimethyl ether (3 mL) and water (1.5 mL) was heated...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Ether
c1c[nH]c2cnncc12.C1CCCC1
c1ccccc1.c1ccccc1.c1c[nH]c2cnncc12.C1CCCC1
c1ccccc1.c1ccccc1.c1c[nH]c2cnncc12.C1CCCC1
Br-
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.O.COCCOC
85
null
Nc1nncc2c1c(Br)cn2C1CCCC1>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.O.COCCOC>Nc1nncc2c1c(-c1ccc(Oc3ccccc3)cc1)cn2C1CCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9dc90570bed3454eaea2d745c410f728
CC(C)c1cccc(B(O)O)c1.Clc1cnccn1>>CC(C)c1cccc(-c2cnccn2)c1
C(C)(C)C=1C=C(C=CC1)B(O)O.ClC1=NC=CN=C1>>C(C)(C)C=1C=C(C=CC1)C1=NC=CN=C1
OB(O)[c:8]1[cH:7][cH:6][cH:5][c:4]([CH:2]([CH3:1])[CH3:3])[cH:15]1.Cl[c:9]1[cH:10][n:11][cH:12][cH:13][n:14]1>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][c:8](-[c:9]2[cH:10][n:11][cH:12][cH:13][n:14]2)[cH:15]1
CC(C)c1cccc(B(O)O)c1.Clc1cnccn1
CC(C)c1cccc(-c2cnccn2)c1
null
C1=CC=C(C=C1)P(CCP(C2=CC=CC=C2)C3=CC=CC=C3)C4=CC=CC=C4.C1=CC=C(C=C1)P(CCP(C2=CC=CC=C2)C3=CC=CC=C3)C4=CC=CC=C4.[Pd]
C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
f4f2599a1f2d23f122d9e68430d5dc3c8a9f800f7adcc4136d8b17b1c1c7d091
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cnccn2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1.O-B(-O)-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:10]:[c:11]>>[c:9]:[c:8]:[c;H0;D3;+0:7](-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1):[c:10]:[c:11]
null
[]
80
CELSIUS
null
null
To a solution of commercial 3-isopropyl-benzene boronic acid (1.0 g) in a 2:2:1 mixture of toluene/1M Na2CO3/EtOH (122 mL), at r.t.,2-chloropyrazine (599 μL) and the bis[1.2-bis(diphenylphosphino)ethane]-palladium(0) catalyst (110 mg) were added. The reaction mixture was heated at 80° C. for 3 hr. It was then cooled do...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1cnccn1
c1ccccc1.c1cnccn1
c1ccccc1.c1cnccn1
HCl.B
C1=CC=C(C=C1)P(CCP(C2=CC=CC=C2)C3=CC=CC=C3)C4=CC=CC=C4.C1=CC=C(C=C1)P(CCP(C2=CC=CC=C2)C3=CC=CC=C3)C4=CC=CC=C4.[Pd].C1(=CC=CC=C1)C
80
null
CC(C)c1cccc(B(O)O)c1.Clc1cnccn1>C1=CC=C(C=C1)P(CCP(C2=CC=CC=C2)C3=CC=CC=C3)C4=CC=CC=C4.C1=CC=C(C=C1)P(CCP(C2=CC=CC=C2)C3=CC=CC=C3)C4=CC=CC=C4.[Pd].C1(=CC=CC=C1)C>CC(C)c1cccc(-c2cnccn2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6ed8d70bbdac4fe6b1078c53aeb4a3c9
Cc1cc(F)ccc1-c1cnccn1>>Cc1cc(F)ccc1C1CNCCN1
FC1=CC(=C(C=C1)C1=NC=CN=C1)C.Cl>>Cl.FC1=CC(=C(C=C1)C1NCCNC1)C
[CH3:1][c:2]1[cH:3][c:4]([F:5])[cH:6][cH:7][c:8]1-[c:9]1[cH:10][n:11][cH:12][cH:13][n:14]1>>[CH3:1][c:2]1[cH:3][c:4]([F:5])[cH:6][cH:7][c:8]1[CH:9]1[CH2:10][NH:11][CH2:12][CH2:13][NH:14]1
Cc1cc(F)ccc1-c1cnccn1
Cc1cc(F)ccc1C1CNCCN1
null
[OH-].[OH-].[Pd+2]
CCO
Reduction
OtherReaction
e72d5c9669dbcc55202ef34c029b3b23b6c11bcbe31d528c7e902f249a9de774
37c66050709a4b09cbaa1fadc57d86c6aebd0e9d91c855b62287cbfd7cec4ba8
c1ccc(C2CNCCN2)cc1
[C;D1;H3:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[c;H0;D3;+0:5]1:[cH;D2;+0:6]:[n;H0;D2;+0:7]:[cH;D2;+0:8]:[cH;D2;+0:9]:[n;H0;D2;+0:10]:1):[c:11]:[c:12]>>[C;D1;H3:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[CH;D3;+0:5]1-[CH2;D2;+0:6]-[NH;D2;+0:7]-[CH2;D2;+0:8]-[CH2;D2;+0:9]-[NH;D2;+0:10]-1):[c:11]:[c:12]
null
[]
null
null
null
null
2-(4-Fluoro-2-methyl-phenyl)-pyrazine (0.3 g) dissolved in EtOH 95% (20 mL) and 37% HCl (0.2 mL) was hydrogenated at 5 atm. for 4 hr, in the presence of 20% Pd(OH)2/C (30 mg) as catalyst. The catalyst was filtered off and the solvent was evaporated. The crude residue was triturated in MeOH/AcOEt (5 mL/15 mL) to obtain ...
10.6084/m9.figshare.5104873.v1
null
null
Secondary amine.Secondary amine
c1cnccn1
C1CNCCN1
c1ccccc1.C1CNCCN1
null
[OH-].[OH-].[Pd+2].CCO
null
null
Cc1cc(F)ccc1-c1cnccn1>[OH-].[OH-].[Pd+2].CCO>Cc1cc(F)ccc1C1CNCCN1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-42dec859f6094151b0c7725b2666b1ad
O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl.O=C1NCCNC1c1ccccc1>>O=C1NCCN(C(=O)Cl)C1c1ccccc1
ClC(Cl)(OC(OC(Cl)(Cl)Cl)=O)Cl.C1(=CC=CC=C1)C1C(NCCN1)=O>>O=C1C(N(CCN1)C(=O)Cl)C1=CC=CC=C1
ClC(Cl)(Cl)O[C:7](OC(Cl)(Cl)[Cl:9])=[O:8].[O:1]=[C:2]1[NH:3][CH2:4][CH2:5][NH:6][CH:10]1[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[O:1]=[C:2]1[NH:3][CH2:4][CH2:5][N:6]([C:7](=[O:8])[Cl:9])[CH:10]1[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl.O=C1NCCNC1c1ccccc1
O=C1NCCN(C(=O)Cl)C1c1ccccc1
null
null
C(Cl)Cl
Acylation
OtherReaction
e42e57261b542adf323d2424161de7351c671a80c841d9853044e323ae3b735d
c5674cad8f50e137418323e673c87f500d3f14758d6a3111a9ca9e5c866850a2
O=C1NCCNC1c1ccccc1
Cl-C(-Cl)(-Cl)-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-O-C(-Cl)(-Cl)-[Cl;H0;D1;+0:3].[O;D1;H0:4]=[C:5]1-[#7:6]-[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-1-[c:11]>>[Cl;H0;D1;+0:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:9]1-[C:8]-[C:7]-[#7:6]-[C:5](=[O;D1;H0:4])-[C:10]-1-[c:11]
56.4
[{"value": 56.4, "product": "O=C1C(N(CCN1)C(=O)Cl)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a stirred solution of triphosgene (0.558 g) in DCM (10 ml) pyridine (0.46 mL) was added at 0° C. and, after 10 min, 3-phenyl-piperazine-2-one (1 g). The ice bath was removed and the mixture was stirred at room temperature overnight. The mixture was concentrated and the product was purified by flash chromatography (C...
10.6084/m9.figshare.5104873.v1
null
Trichloro group.Trichloro group.Carbonic Ester.Secondary amine
Acyl halide.Tertiary amide
C1CNCCN1
C1C[NH]CCN1
C1C[NH]CCN1.c1ccccc1
HCl
C(Cl)Cl
null
8
O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl.O=C1NCCNC1c1ccccc1>C(Cl)Cl>O=C1NCCN(C(=O)Cl)C1c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-85427b73764646c9b92cca818977921d
C[Si](C)(C)C=[N+]=[N-].O=C(O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1>>COC(=O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
C[Si](C)(C)C=[N+]=[N-].FC(C=1C=C(C(=O)O)C=C(C1)C(F)(F)F)(F)F>>COC(C1=CC(=CC(=C1)C(F)(F)F)C(F)(F)F)=O
C[Si](C)(C)[CH:1]=[N+]=[N-].[OH:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([C:8]([F:9])([F:10])[F:11])[cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([C:8]([F:9])([F:10])[F:11])[cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18]1
C[Si](C)(C)C=[N+]=[N-].O=C(O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
COC(=O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
null
null
C1(=CC=CC=C1)C.CO
Heteroatom Alkylation and Arylation
O-alkylation of carboxylic acids with diazo compounds
39589be0e9a30df66714fe618d22a8ac0fb24901dbf2ead1ab33e31556c7ac64
8b539baf7aeb5ab868833e33306bad77200a853d562904197e13de2e27e229d7
c1ccccc1
C-[Si](-C)(-C)-[CH;D2;+0:1]=[N+]=[N-].[O;D1;H0:2]=[C:3](-[OH;D1;+0:4])-[c:5]>>[CH3;D1;+0:1]-[O;H0;D2;+0:4]-[C:3](=[O;D1;H0:2])-[c:5]
null
[]
0
CELSIUS
1
HOUR
Trimethylsilyldiazomethane (11.5 mL) was added drop-wise to a solution of 3,5-bis-(trifluoromethyl)benzoic acid (2 g) in dry toluene (20 mL) and methanol (0.5 mL) previously cooled to 0° C. under a nitrogen atmosphere. The solution was stirred at r.t. for 1 hr, then concentrated in vacuo to give 3,5-bis-(trifluoromethy...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Diazo.Silyl protective group
Ester
null
null
c1ccccc1
Other
C1(=CC=CC=C1)C.CO
0
1
C[Si](C)(C)C=[N+]=[N-].O=C(O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1>C1(=CC=CC=C1)C.CO>COC(=O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8ae11a41d865478e840482f4273371ed
COC(=O)C(C)(C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1>>CC(C)(C(=O)O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
Cl.FC(C=1C=C(C=C(C1)C(F)(F)F)C(C(=O)OC)(C)C)(F)F.[OH-].[K+]>>FC(C=1C=C(C=C(C1)C(F)(F)F)C(C(=O)O)(C)C)(F)F
C[O:6][C:4]([C:2]([CH3:1])([CH3:3])[c:7]1[cH:8][c:9]([C:10]([F:11])([F:12])[F:13])[cH:14][c:15]([C:16]([F:17])([F:18])[F:19])[cH:20]1)=[O:5]>>[CH3:1][C:2]([CH3:3])([C:4](=[O:5])[OH:6])[c:7]1[cH:8][c:9]([C:10]([F:11])([F:12])[F:13])[cH:14][c:15]([C:16]([F:17])([F:18])[F:19])[cH:20]1
COC(=O)C(C)(C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
CC(C)(C(=O)O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
null
null
CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccccc1
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]
null
[]
null
null
null
null
A solution of 2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionic acid, methyl ester (intermediate 69-184 mg) and potassium hydroxide (131 mg) in MeOH (2.5 mL) was heated to reflux for 1 hour, then it was allowed to cool to r.t. and acidified to pH=3 with 10% hydrochloric acid solution and extracted with AcOEt (2×10 ...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1
Other
CO
null
null
COC(=O)C(C)(C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1>CO>CC(C)(C(=O)O)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-35bdd3b1dd06456e91d478cc0db0ae3e
Cc1cc(F)ccc1[C@H]1CNCCN1.O=C(Cl)OCc1ccccc1>>Cc1cc(F)ccc1[C@H]1CN(C(=O)OCc2ccccc2)CCN1
C(C1=CC=CC=C1)OC(=O)Cl.Cl.Cl.FC1=CC(=C(C=C1)[C@@H]1NCCNC1)C>>C(C1=CC=CC=C1)OC(=O)N1C[C@@H](NCC1)C1=C(C=C(C=C1)F)C
[CH3:1][c:2]1[cH:3][c:4]([F:5])[cH:6][cH:7][c:8]1[C@H:9]1[CH2:10][NH:11][CH2:22][CH2:23][NH:24]1.Cl[C:12](=[O:13])[O:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1>>[CH3:1][c:2]1[cH:3][c:4]([F:5])[cH:6][cH:7][c:8]1[C@H:9]1[CH2:10][N:11]([C:12](=[O:13])[O:14][CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[C...
Cc1cc(F)ccc1[C@H]1CNCCN1.O=C(Cl)OCc1ccccc1
Cc1cc(F)ccc1[C@H]1CN(C(=O)OCc2ccccc2)CCN1
null
null
C(Cl)Cl
Protection
N-alkylation of secondary amines with alkyl halides
4451143905f811374b7e4cef978840c2bcbd908fec8f94e9f20bbc2686e59370
d86dc1e6d0e089b3444b62ddfcf4c4822bdac4b60e628553036562518c29adcd
O=C(OCc1ccccc1)N1CCN[C@@H](c2ccccc2)C1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C:4].[#7:5]1-[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]-1>>[C:4]-[#8:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:8]1-[C:9]-[C:10]-[#7:5]-[C:6]-[C:7]-1
null
[]
0
CELSIUS
2
HOUR
A solution of benzylchloroformate (376 μL) in dry DCM (20 mL) was added drop-wise to a solution of the 2-(S)-(4-fluoro-2-methyl-phenyl)-piperazine dihydrochloride (700 mg) and TEA (1.1 mL) in DCM (30 mL) previously cooled to 0° C. under a nitrogen atmosphere. The mixture was stirred at r.t. for 2 hrs, then washed with ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether.Secondary amine
Carbamic ester
C1CNCCN1
C1CNCC[NH]1
c1ccccc1.C1CNCC[NH]1.c1ccccc1
HCl
C(Cl)Cl
0
2
Cc1cc(F)ccc1[C@H]1CNCCN1.O=C(Cl)OCc1ccccc1>C(Cl)Cl>Cc1cc(F)ccc1[C@H]1CN(C(=O)OCc2ccccc2)CCN1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-694454ae10164c309a818a8eeef7f6af
CC(C)I.COC(=O)Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1>>COC(=O)C(c1cc(C(F)(F)F)cc(C(F)(F)F)c1)C(C)C
C(C)(C)I.C[Si](C)(C)[N-][Si](C)(C)C.[Na+].COC(CC1=CC(=CC(=C1)C(F)(F)F)C(F)(F)F)=O.C(C)(C)I>>COC(C(C(C)C)C1=CC(=CC(=C1)C(F)(F)F)C(F)(F)F)=O
I[CH:20]([CH3:21])[CH3:22].[CH3:1][O:2][C:3](=[O:4])[CH2:5][c:6]1[cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[cH:13][c:14]([C:15]([F:16])([F:17])[F:18])[cH:19]1>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([c:6]1[cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[cH:13][c:14]([C:15]([F:16])([F:17])[F:18])[cH:19]1)[CH:20]([CH3:21])[CH3:22]
CC(C)I.COC(=O)Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1
COC(=O)C(c1cc(C(F)(F)F)cc(C(F)(F)F)c1)C(C)C
null
null
C1CCOC1
C-C Coupling
OtherReaction
8c44d57f8486d6bee1a0b83f6845f011ce41bc47981bdbe8dc66352f860486a8
ae23b78d8cc9afe1235c3056fa58900d3a27e232dc891dd767f4195ab4ddcbb6
c1ccccc1
I-[CH;D3;+0:1](-[C;D1;H3:2])-[C;D1;H3:3].[C;D1;H3:4]-[#8:5]-[C:6](=[O;D1;H0:7])-[CH2;D2;+0:8]-[c:9](:[c:10]):[c:11]>>[C;D1;H3:4]-[#8:5]-[C:6](=[O;D1;H0:7])-[CH;D3;+0:8](-[CH;D3;+0:1](-[C;D1;H3:2])-[C;D1;H3:3])-[c:9](:[c:10]):[c:11]
null
[]
0
CELSIUS
30
MINUTE
Sodium bis(trimethylsilyl) amide (1.0M in THF—177 μL) was added drop-wise to a solution of (3,5-bis-trifluoromethyl-phenyl)-acetic acid methyl ester (389 mg) in dry THF (2 mL) at 0° C., under nitrogen atmosphere. After ten minutes, isopropyl iodide (143 μL) was added and the reaction mixture was stirred at 0° C. for 30...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Ester
Ester
null
null
c1ccccc1
HI
C1CCOC1
0
0.5
CC(C)I.COC(=O)Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1>C1CCOC1>COC(=O)C(c1cc(C(F)(F)F)cc(C(F)(F)F)c1)C(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3075e11c84e842c1acd56b5278c1e549
CN.O=Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1>>CN=Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1
FC(C=1C=C(C=O)C=C(C1)C(F)(F)F)(F)F.CN>>FC(C=1C=C(C=NC)C=C(C1)C(F)(F)F)(F)F
[CH3:1][NH2:2].O=[CH:3][c:4]1[cH:5][c:6]([C:7]([F:8])([F:9])[F:10])[cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17]1>>[CH3:1][N:2]=[CH:3][c:4]1[cH:5][c:6]([C:7]([F:8])([F:9])[F:10])[cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17]1
CN.O=Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1
CN=Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Addition of primary amines to aldehydes/thiocarbonyls
d409dfd3247abb6c1b1364aec380d25720f21e374fd2124063f2d2ce54d31c4f
9b341044a5a058244685b0b956d33f593ccdcd7346fa1d8d7b98a302fd35b8a2
c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C;D1;H3:5]-[NH2;D1;+0:6]>>[C;D1;H3:5]-[N;H0;D2;+0:6]=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
8
HOUR
A solution of 3,5-bis(trifluoromethyl)-benzaldehyde (412 μL) in dry THF (5 mL) was added dropwise to a solution of methylamine (2M in MeOH—3.12 mL) in dry THF (5 mL) at 23° C. under a nitrogen atmosphere. The reaction mixture was stirred overnight, then the solvent was evaporated in vacuo to give the title compound (38...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine
Substituted imine
null
null
c1ccccc1
HO-
C1CCOC1
null
8
CN.O=Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1>C1CCOC1>CN=Cc1cc(C(F)(F)F)cc(C(F)(F)F)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-891a97e306d4495992d9116c500348f2
Cc1cc(F)ccc1[C@H]1C(=O)NCCN1C(=O)N(C)[C@H](C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1>>Cc1cc(F)ccc1[C@H]1CNCCN1C(=O)N(C)[C@H](C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
C(=O)(O)[O-].[Na+].FC(C=1C=C(C=C(C1)C(F)(F)F)[C@@H](C)N(C(=O)N1[C@H](C(NCC1)=O)C1=C(C=C(C=C1)F)C)C)(F)F.B.C1CCOC1.Cl>>FC(C=1C=C(C=C(C1)C(F)(F)F)[C@@H](C)N(C(=O)N1[C@H](CNCC1)C1=C(C=C(C=C1)F)C)C)(F)F
O=[C:10]1[C@H:9]([c:8]2[c:2]([CH3:1])[cH:3][c:4]([F:5])[cH:6][cH:7]2)[N:14]([C:15](=[O:16])[N:17]([CH3:18])[C@H:19]([CH3:20])[c:21]2[cH:22][c:23]([C:24]([F:25])([F:26])[F:27])[cH:28][c:29]([C:30]([F:31])([F:32])[F:33])[cH:34]2)[CH2:13][CH2:12][NH:11]1>>[CH3:1][c:2]1[cH:3][c:4]([F:5])[cH:6][cH:7][c:8]1[C@H:9]1[CH2:10][N...
Cc1cc(F)ccc1[C@H]1C(=O)NCCN1C(=O)N(C)[C@H](C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
Cc1cc(F)ccc1[C@H]1CNCCN1C(=O)N(C)[C@H](C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
null
null
O.C1CCOC1
Reduction
Reduction of secondary amides to amines
b51112e31d2a8841c3f8da7b8557990b065c14a7b2c0de6d1b1989d541f5c0bd
ab40188eef2f825df7003af0ffae31d0ce53d126542122535627d3d354cbc9fe
O=C(NCc1ccccc1)N1CCNC[C@@H]1c1ccccc1
O=[C;H0;D3;+0:1]1-[#7:2]-[C:3]-[C:4]-[#7:5](-[C:6](-[#7:7])=[O;D1;H0:8])-[C:9]-1-[c:10]>>[#7:7]-[C:6](=[O;D1;H0:8])-[#7:5]1-[C:4]-[C:3]-[#7:2]-[CH2;D2;+0:1]-[C:9]-1-[c:10]
57.4
[{"value": 57.4, "product": "FC(C=1C=C(C=C(C1)C(F)(F)F)[C@@H](C)N(C(=O)N1[C@H](CNCC1)C1=C(C=C(C=C1)F)C)C)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of intermediate 40a (15.6 g) in anhydrous THF (94 ml), at 0° C., under N2, BH3.THF 1M/THF (154 ml) was added. The solution was heated at reflux for 3 hr. HCl 37% (54 ml) was slowly added maintaining the reaction mixture in an ice-bath and the reaction mixture was stirred at rt for 1 hr. Water was then add...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
null
C1CNCC[NH]1
C1C[NH]CCN1
c1ccccc1.C1C[NH]CCN1.c1ccccc1
Other
O.C1CCOC1
null
1
Cc1cc(F)ccc1[C@H]1C(=O)NCCN1C(=O)N(C)[C@H](C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1>O.C1CCOC1>Cc1cc(F)ccc1[C@H]1CNCCN1C(=O)N(C)[C@H](C)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a0ec281597b743318293b3929a95087b
COc1ccc(-c2cc3c(n2-c2ccccc2C)CCN(Cc2ccccc2)C3)cc1>>COc1ccc(-c2cc3c(n2-c2ccccc2C)CCNC3)cc1
C(C1=CC=CC=C1)N1CC2=C(CC1)N(C(=C2)C2=CC=C(C=C2)OC)C2=C(C=CC=C2)C>>COC1=CC=C(C=C1)C1=CC=2CNCCC2N1C1=C(C=CC=C1)C
c1ccc(C[N:21]2[CH2:20][CH2:19][c:10]3[c:9]([cH:8][c:7](-[c:6]4[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:24][cH:23]4)[n:11]3-[c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[CH3:18])[CH2:22]2)cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[CH3:18])[CH2:19][CH2:20]...
COc1ccc(-c2cc3c(n2-c2ccccc2C)CCN(Cc2ccccc2)C3)cc1
COc1ccc(-c2cc3c(n2-c2ccccc2C)CCNC3)cc1
null
[OH-].[OH-].[Pd+2]
O1CCCC1.CO
Deprotection
Hydrogenolysis of tertiary amines
a30eaa236a81ef147f5f28e4d833ab14e33a5d35b9de7b2cf9c009f8aa08011d
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
c1ccc(-c2cc3c(n2-c2ccccc2)CCNC3)cc1
[#7;a:1]:[c:2]1:[c:3]-[C:4]-[N;H0;D3;+0:5](-C-c2:c:c:c:c:c:2)-[C:6]-[C:7]-1>>[#7;a:1]:[c:2]1:[c:3]-[C:4]-[NH;D2;+0:5]-[C:6]-[C:7]-1
98
[{"value": 98.0, "product": "COC1=CC=C(C=C1)C1=CC=2CNCCC2N1C1=C(C=CC=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.5, "product": "COC1=CC=C(C=C1)C1=CC=2CNCCC2N1C1=C(C=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
5-Benzyl-2-(4-methoxyphenyl)-1-(2-methylphenyl)4,5,6,7-tetrahydro-1H-pyrrolo[3,2-c]pyridine (5.6 g, 14 mmol; prepared by methods as described in Example 1) was added to a suspension of palladium hydroxide on carbon (20%, 1.52 g, 2 mmol) in dry methanol (130 mL) and tetrahydrofuran (100 mL) under argon. The mixture was ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.c1cc2c(n1)CCNC2
c1cc2c([nH]1)CCNC2
c1ccccc1.c1ccccc1.c1cc2c([nH]1)CCNC2
Other
[OH-].[OH-].[Pd+2].O1CCCC1.CO
null
8
COc1ccc(-c2cc3c(n2-c2ccccc2C)CCN(Cc2ccccc2)C3)cc1>[OH-].[OH-].[Pd+2].O1CCCC1.CO>COc1ccc(-c2cc3c(n2-c2ccccc2C)CCNC3)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7fc9c81abdff47de8db2aee8312afd71
Cc1c2c(n(-c3ccccc3Cl)c1-c1ccc(Cl)cc1)CCNC2=O>>Cc1c2c(n(-c3ccccc3Cl)c1-c1ccc(Cl)cc1)CCNC2
ClC1=C(C=CC=C1)N1C(=C(C=2C(NCCC21)=O)C)C2=CC=C(C=C2)Cl.CO>>ClC1=C(C=CC=C1)N1C(=C(C=2CNCCC21)C)C2=CC=C(C=C2)Cl
O=[C:24]1[c:3]2[c:2]([CH3:1])[c:13](-[c:14]3[cH:15][cH:16][c:17]([Cl:18])[cH:19][cH:20]3)[n:5](-[c:6]3[cH:7][cH:8][cH:9][cH:10][c:11]3[Cl:12])[c:4]2[CH2:21][CH2:22][NH:23]1>>[CH3:1][c:2]1[c:3]2[c:4]([n:5](-[c:6]3[cH:7][cH:8][cH:9][cH:10][c:11]3[Cl:12])[c:13]1-[c:14]1[cH:15][cH:16][c:17]([Cl:18])[cH:19][cH:20]1)[CH2:21]...
Cc1c2c(n(-c3ccccc3Cl)c1-c1ccc(Cl)cc1)CCNC2=O
Cc1c2c(n(-c3ccccc3Cl)c1-c1ccc(Cl)cc1)CCNC2
null
null
O1CCCC1
Reduction
Reduction of secondary amides to amines
437c5db55f5f849f6a4e5360499407e96999484d6cddd734b0881e250538cd04
ab40188eef2f825df7003af0ffae31d0ce53d126542122535627d3d354cbc9fe
c1ccc(-c2cc3c(n2-c2ccccc2)CCNC3)cc1
O=[C;H0;D3;+0:1]1-[#7:2]-[C:3]-[C:4]-[c:5]2:[#7;a:6](-[c:7]):[c:8]:[c:9]:[c:10]:2-1>>[c:7]-[#7;a:6]1:[c:8]:[c:9]:[c:10]2:[c:5]:1-[C:4]-[C:3]-[#7:2]-[CH2;D2;+0:1]-2
34.8
[{"value": 34.8, "product": "ClC1=C(C=CC=C1)N1C(=C(C=2CNCCC21)C)C2=CC=C(C=C2)Cl", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 1-(2-chlorophenyl)-2-(4-chlorophenyl)-3-methyl-1,5,6,7-tetrahydro-4H-pyrrolo[3,2-c]pyridin-4-one (2.84 g, 7.64 mmol, prepared as in Scheme 2 and in a similar manner to Example 22) in tetrahydrofuran (38 mL) was added borane-tetrahydrofuran complex (1 M, 76 mL) at 0° C. over 20 minutes. The mixture was ...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
null
C1NCCc2[nH]ccc21
c1cc2c([nH]1)CCNC2
c1ccccc1.c1ccccc1.c1cc2c([nH]1)CCNC2
Other
O1CCCC1
null
null
Cc1c2c(n(-c3ccccc3Cl)c1-c1ccc(Cl)cc1)CCNC2=O>O1CCCC1>Cc1c2c(n(-c3ccccc3Cl)c1-c1ccc(Cl)cc1)CCNC2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6e6784a81a91463a8f895bb1e9274f2a
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.CS(=O)(=O)Cl>>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(S(C)(=O)=O)C3)cc1
ClC1=C(C=CC=C1)N1C(=CC=2CNCCC21)C2=CC=C(C=C2)OC.CS(=O)(=O)Cl>>ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)S(=O)(=O)C)C2=CC=C(C=C2)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[Cl:18])[CH2:19][CH2:20][NH:21][CH2:26]3)[cH:27][cH:28]1.Cl[S:22]([CH3:23])(=[O:24])=[O:25]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[Cl...
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.CS(=O)(=O)Cl
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(S(C)(=O)=O)C3)cc1
null
null
ClCCl
Acylation
Sulfonamide synthesis (Schotten-Baumann) secondary amine
3a2568ea67a50ab5e23bc11a629b46235140e4e3e9c40d4154c620903e696245
b7aca5a5d690b0846685a854bc946849e1041bfc3965161290b5ffb2821af09e
c1ccc(-c2cc3c(n2-c2ccccc2)CCNC3)cc1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#7;a:5]:[c:6]1:[c:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]-1>>[#7;a:5]:[c:6]1:[c:7]-[C:8]-[N;H0;D3;+0:9](-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4])-[C:10]-[C:11]-1
40
[{"value": 40.0, "product": "ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)S(=O)(=O)C)C2=CC=C(C=C2)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
To an 8-mL vial charged with piperidinomethyl polystyrene (3.57 mmol/g, 99.2 mg, 0.354 mmol) and a solution of 1-(2-chlorophenyl)-2-(4-methoxyphenyl)-4,5,6,7-tetrahydro-1H-pyrrolo[3,2-c]pyridine (Example 2), 40.0 mg, 0.118 mmol) in 4 mL dichloromethane was added methanesulfonyl chloride (18.2 μL, 0.236 mmol). The react...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Sulfonyl halide
Tertiary amine
c1cc2c([nH]1)CCNC2
c1cc2c([nH]1)CCNC2
c1ccccc1.c1ccccc1.c1cc2c([nH]1)CCNC2
HCl
ClCCl
null
4
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.CS(=O)(=O)Cl>ClCCl>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(S(C)(=O)=O)C3)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6799d787040d4ac2895b8f40a6daa6ba
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.O=C(Cl)c1cccc(Cl)c1>>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(C(=O)c2cccc(Cl)c2)C3)cc1
ClC1=C(C=CC=C1)N1C(=CC=2CNCCC21)C2=CC=C(C=C2)OC.ClC=1C=C(C(=O)Cl)C=CC1>>ClC=1C=C(C(=O)N2CC3=C(CC2)N(C(=C3)C3=CC=C(C=C3)OC)C3=C(C=CC=C3)Cl)C=CC1
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[Cl:18])[CH2:19][CH2:20][NH:21][CH2:31]3)[cH:32][cH:33]1.Cl[C:22](=[O:23])[c:24]1[cH:25][cH:26][cH:27][c:28]([Cl:29])[cH:30]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:...
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.O=C(Cl)c1cccc(Cl)c1
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(C(=O)c2cccc(Cl)c2)C3)cc1
null
null
ClCCl
Acylation
N-alkylation of secondary amines with alkyl halides
29af23b4550a2433d66824e283c10763b6d571f521c33e8dc5eb8903d9dd7366
96cb0a2fed10552c5770a45a2d6523b47ac3e38928b4a9c698d8577451182dcd
O=C(c1ccccc1)N1CCc2c(cc(-c3ccccc3)n2-c2ccccc2)C1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[#7;a:6]:[c:7]1:[c:8]-[C:9]-[NH;D2;+0:10]-[C:11]-[C:12]-1>>[#7;a:6]:[c:7]1:[c:8]-[C:9]-[N;H0;D3;+0:10](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5])-[C:11]-[C:12]-1
74
[{"value": 74.0, "product": "ClC=1C=C(C(=O)N2CC3=C(CC2)N(C(=C3)C3=CC=C(C=C3)OC)C3=C(C=CC=C3)Cl)C=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73.8, "product": "ClC=1C=C(C(=O)N2CC3=C(CC2)N(C(=C3)C3=CC=C(C=C3)OC)C3=C(C=CC=C3)Cl)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To an 8-mL vial charged with piperidinomethyl polystyrene (3.57 mmol/g, 198.4 mg, 0.708 mmol) and a solution of 1-(2-chlorophenyl)-2-(4-methoxyphenyl)-4,5,6,7-tetrahydro-1H-pyrrolo[3,2-c]pyridine (Example 2, 80.0 mg, 0.236 mmol) in 3 mL dichloromethane was added 3-chlorobenzoyl chloride (62.0 mg, 0.0.54 mmol). The reac...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary amine
Tertiary amide
c1cc2c([nH]1)CCNC2
c1cc2c([nH]1)CCNC2
c1ccccc1.c1ccccc1.c1cc2c([nH]1)CCNC2.c1ccccc1
HCl
ClCCl
null
3
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.O=C(Cl)c1cccc(Cl)c1>ClCCl>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(C(=O)c2cccc(Cl)c2)C3)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6157255225ff4b5cbcd857cbe125149b
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.N#Cc1ccc(F)cc1>>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(c2ccc(C#N)cc2)C3)cc1
O.ClC1=C(C=CC=C1)N1C(=CC=2CNCCC21)C2=CC=C(C=C2)OC.C(=O)([O-])[O-].[K+].[K+].FC1=CC=C(C#N)C=C1>>ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)C2=CC=C(C#N)C=C2)C2=CC=C(C=C2)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[Cl:18])[CH2:19][CH2:20][NH:21][CH2:30]3)[cH:31][cH:32]1.F[c:22]1[cH:23][cH:24][c:25]([C:26]#[N:27])[cH:28][cH:29]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14]...
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.N#Cc1ccc(F)cc1
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(c2ccc(C#N)cc2)C3)cc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation secondary amine
98bcac89b32aa2b2766de9cac3f112509802dda7c2f349793518bb59d21a12ab
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc(-c2cc3c(n2-c2ccccc2)CCN(c2ccccc2)C3)cc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[#7;a:6]:[c:7]1:[c:8]-[C:9]-[NH;D2;+0:10]-[C:11]-[C:12]-1>>[#7;a:6]:[c:7]1:[c:8]-[C:9]-[N;H0;D3;+0:10](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5])-[C:11]-[C:12]-1
43.1
[{"value": 43.0, "product": "ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)C2=CC=C(C#N)C=C2)C2=CC=C(C=C2)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 43.1, "product": "ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)C2=CC=C(C#N)C=C2)C2=CC=C(C=C2)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
130
CELSIUS
48
HOUR
To a suspension of 1-(2-chlorophenyl)-2-(4-methoxyphenyl)-4,5,6,7-tetrahydro-1H-pyrrolo[3,2-c]pyridine (Example 2, 80.0 mg, 0.236 mmol) and K2CO3 (97.9 mg, 0.708 mmol) in 2 mL DMF was added 4-fluorobenzonitrile (86.0 mg, 0.472 mmol) under argon. The mixture was heated at 130° C. with stirring for 48 h. The mixture was ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
c1cc2c([nH]1)CCNC2.c1ccccc1
c1cc2c([nH]1)CCNC2.c1ccccc1
c1ccccc1.c1ccccc1.c1cc2c([nH]1)CCNC2.c1ccccc1
HF
CN(C)C=O
130
48
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.N#Cc1ccc(F)cc1>CN(C)C=O>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(c2ccc(C#N)cc2)C3)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-59c2d44fd8294022b89c4269dbe6bbe8
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.O=Cc1ccc(F)cc1>>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(Cc2ccc(F)cc2)C3)cc1
ClC1=C(C=CC=C1)N1C(=CC=2CNCCC21)C2=CC=C(C=C2)OC.FC1=CC=C(C=O)C=C1.C(C)(=O)O.[BH-](OC(=O)C)(OC(=O)C)OC(=O)C.[Na+].[OH-].[Na+]>>ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)CC2=CC=C(C=C2)F)C2=CC=C(C=C2)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[Cl:18])[CH2:19][CH2:20][NH:21][CH2:30]3)[cH:31][cH:32]1.O=[CH:22][c:23]1[cH:24][cH:25][c:26]([F:27])[cH:28][cH:29]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14...
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.O=Cc1ccc(F)cc1
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(Cc2ccc(F)cc2)C3)cc1
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
reductive amination
646a2fc9876a66e5c3dd23cf2d7c8f8318244c05a5ce4ae33e5c1213861b4527
2d03f38884b1fbb0c0d6e6f2de31afb25102fec87f347c3a123e064c1bfef0ad
c1ccc(CN2CCc3c(cc(-c4ccccc4)n3-c3ccccc3)C2)cc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[#7;a:5]:[c:6]1:[c:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]-1>>[#7;a:5]:[c:6]1:[c:7]-[C:8]-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10]-[C:11]-1
97.6
[{"value": 97.0, "product": "ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)CC2=CC=C(C=C2)F)C2=CC=C(C=C2)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.6, "product": "ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)CC2=CC=C(C=C2)F)C2=CC=C(C=C2)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 1-(2-chlorophenyl)-2-(4-methoxyphenyl)-4,5,6,7-tetrahydro-1H-pyrrolo[3,2-c]pyridine (Example 2, 677.7 mg, 0.50 mmol), 4-fluorobenzaldehyde (0.13 mL, 0.60 mmol), acetic acid (0.03 mL, 0.60 mmol), and NaBH(OAc)3 (148.4 mg, 0.70 mmol) in methylene chloride (15 mL) was stirred at rt for 24 h. Sodium hydroxide...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine
Tertiary amine
c1cc2c([nH]1)CCNC2
c1cc2c([nH]1)CCNC2
c1ccccc1.c1ccccc1.c1cc2c([nH]1)CCNC2.c1ccccc1
Other
C(Cl)Cl
null
null
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1.O=Cc1ccc(F)cc1>C(Cl)Cl>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN(Cc2ccc(F)cc2)C3)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-293f4bd587b248f481c424a748897cdb
C1CCC2OC2C1.COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1>>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN([C@@H]2CCCC[C@H]2O)C3)cc1
ClC1=C(C=CC=C1)N1C(=CC=2CNCCC21)C2=CC=C(C=C2)OC.C12C(CCCC1)O2.C(C)N(CC)CC>>ClC1=C(C=CC=C1)N1C(=CC=2CN(CCC21)[C@H]2[C@@H](CCCC2)O)C2=CC=C(C=C2)OC
[CH:22]12[CH2:23][CH2:24][CH2:25][CH2:26][CH:27]1[O:28]2.[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[Cl:18])[CH2:19][CH2:20][NH:21][CH2:29]3)[cH:30][cH:31]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]3[c:10]([n:11]2-[c:12]2[cH:13][cH:14][c...
C1CCC2OC2C1.COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1
COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN([C@@H]2CCCC[C@H]2O)C3)cc1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
669763d3d59100f79b0e1c9b6a21e4eb34626c345a144f0a758f4736c3c1a9c1
97e758d6c4c8255d25541eb6c6a6f62e7dc30829ea162ca3392731efabc98a65
c1ccc(-c2cc3c(n2-c2ccccc2)CCN(C2CCCCC2)C3)cc1
[#7;a:1]:[c:2]1:[c:3]-[C:4]-[NH;D2;+0:5]-[C:6]-[C:7]-1.[C:8]1-[C:9]-[C:10]-[C:11]-[CH;D3;+0:12]2-[O;H0;D2;+0:13]-[CH;D3;+0:14]-1-2>>[#7;a:1]:[c:2]1:[c:3]-[C:4]-[N;H0;D3;+0:5](-[C@@H;D3;+0:14]2-[C:8]-[C:9]-[C:10]-[C:11]-[C@H;D3;+0:12]-2-[OH;D1;+0:13])-[C:6]-[C:7]-1
63
[{"value": 63.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 1-(2-chlorophenyl)-2-(4-methoxyphenyl)-4,5,6,7-tetrahydro-1H-pyrrolo[3,2-c]pyridine (Example 2, 500 mg, 1.33 mmol), cyclohexene oxide (1.34 mL, 13.3 mmol), and trietylamine (0.55 mL, 3.99 mmol) in ethanol (14 mL) was heated at reflux for 20 h. The solution was cooled to rt, and evaporated. The residue was...
10.6084/m9.figshare.5104873.v1
null
Ether.Secondary amine
Secondary alcohol.Tertiary amine
C1CCC2OC2C1.c1cc2c([nH]1)CCNC2
c1cc2c([nH]1)CCNC2.C1CCCCC1
c1ccccc1.c1ccccc1.c1cc2c([nH]1)CCNC2.C1CCCCC1
null
C(C)O
null
null
C1CCC2OC2C1.COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCNC3)cc1>C(C)O>COc1ccc(-c2cc3c(n2-c2ccccc2Cl)CCN([C@@H]2CCCC[C@H]2O)C3)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d0cf7eeebaf94d0aba3dad3492e83406
C=CC(=O)OC.NN1CCCCC1>>COC(=O)CCNN1CCCCC1
NN1CCCCC1.C(C=C)(=O)OC>>N1(CCCCC1)NCCC(=O)OC
[CH3:1][O:2][C:3](=[O:4])[CH:5]=[CH2:6].[NH2:7][N:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][CH2:6][NH:7][N:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1
C=CC(=O)OC.NN1CCCCC1
COC(=O)CCNN1CCCCC1
null
null
CO
Heteroatom Alkylation and Arylation
aza-Michael addition primary
4a7280b3eca378a7e174ed7608bea18efb9ff5e7b0de5642dfc83fdcafa072ff
a32db21c2fbc4fea36d992580fcfff2a8264d071438edbd339d759c2c914b63b
C1CCNCC1
[C;D1;H3:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH;D2;+0:5]=[CH2;D1;+0:6].[C:7]-[#7:8](-[NH2;D1;+0:9])-[C:10]>>[C:7]-[#7:8](-[NH;D2;+0:9]-[CH2;D2;+0:6]-[CH2;D2;+0:5]-[C:3](=[O;D1;H0:4])-[#8:2]-[C;D1;H3:1])-[C:10]
50.5
[{"value": 50.5, "product": "N1(CCCCC1)NCCC(=O)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 50.5, "product": "N1(CCCCC1)NCCC(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of 1-aminopiperidine (100 g, 1.00 mol) in dry MeOH (1.00 L) at 0° C., methyl acrylate (99 mL, 1.10 mol) was added dropwise over 2 h. The resulting mixture was stirred overnight at rt. The solvents were evaporated, hexane was added to the residue, and white solid (impurity) was precipitated. The solid was ...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ester.Vinyl
Hydrazine.Ester
null
null
C1CC[NH]CC1
null
CO
null
8
C=CC(=O)OC.NN1CCCCC1>CO>COC(=O)CCNN1CCCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a7f3b81c55c44181a9904755fcdbcc78
CCOC(=O)CC(=O)N(CCC(=O)OC)N1CCCCC1>>CCOC(=O)C1C(=O)CCN(N2CCCCC2)C1=O
C(C)OC(CC(=O)N(CCC(=O)OC)N1CCCCC1)=O.C(=O)([O-])[O-].[Cs+].[Cs+]>>O=C1N(CCC(C1C(=O)OCC)=O)N1CCCCC1
CO[C:7](=[O:8])[CH2:9][CH2:10][N:11]([N:12]1[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]1)[C:18]([CH2:6][C:4]([O:3][CH2:2][CH3:1])=[O:5])=[O:19]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]1[C:7](=[O:8])[CH2:9][CH2:10][N:11]([N:12]2[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]2)[C:18]1=[O:19]
CCOC(=O)CC(=O)N(CCC(=O)OC)N1CCCCC1
CCOC(=O)C1C(=O)CCN(N2CCCCC2)C1=O
null
null
CN(C)C=O.C1CCOC1
Functional Group Interconversion
OtherReaction
076c99fb8e1f07279e9954d28b83a2cf6b3e59e63bbf119695ed51e03379a58f
6f130a746a78d10ca37f94948711de2b0c76f45052ca887b0e681c66276a7764
O=C1CCN(N2CCCCC2)C(=O)C1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]-[#7:5](-[#7:6])-[C:7](=[O;D1;H0:8])-[CH2;D2;+0:9]-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]>>[#7:6]-[#7:5]1-[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH;D3;+0:9](-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13])-[C:7]-1=[O;D1;H0:8]
null
[]
77
CELSIUS
null
null
To a solution of methyl N-(3-ethoxy-3-oxopropanoyl)-N-(1-piperidinyl)-β-alaninate (43 g, 143 mmol) in a mixture of THF (2.26 L) and DMF (1.00 L) was added Cs2CO3 (140 g, 430 mmol). The resulting mixture was heated at reflux (77° C.) for 48 h. The cooled reaction was filtered, and the filtrate was evaporated. The filtra...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Ketone
null
C1CC[NH]CC1
C1CC[NH]CC1.C1CC[NH]CC1
HO-
CN(C)C=O.C1CCOC1
77
null
CCOC(=O)CC(=O)N(CCC(=O)OC)N1CCCCC1>CN(C)C=O.C1CCOC1>CCOC(=O)C1C(=O)CCN(N2CCCCC2)C1=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-68ade4b66e4b4b659a2a112d0fd74d5d
CCOC(=O)C1C(=O)CCN(N2CCCCC2)C1=O>>O=C1CCN(N2CCCCC2)C(=O)C1
O=C1N(CCC(C1C(=O)OCC)=O)N1CCCCC1>>N1(C(CC(CC1)=O)=O)N1CCCCC1
CCOC(=O)[CH:14]1[C:2](=[O:1])[CH2:3][CH2:4][N:5]([N:6]2[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]2)[C:12]1=[O:13]>>[O:1]=[C:2]1[CH2:3][CH2:4][N:5]([N:6]2[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]2)[C:12](=[O:13])[CH2:14]1
CCOC(=O)C1C(=O)CCN(N2CCCCC2)C1=O
O=C1CCN(N2CCCCC2)C(=O)C1
null
null
CC(=O)O
Reduction
Decarboxylation
8fbe6375b12ffe41ffbcdf7408be0ba972c9810d9359e6d6596b942b093a6619
f277909394d9f4e61cc2cdb65fef123102672ca91cfff7f8513cb0baf66138ac
O=C1CCN(N2CCCCC2)C(=O)C1
C-C-O-C(=O)-[CH;D3;+0:1]1-[C:2](=[O;D1;H0:3])-[#7:4](-[#7:5])-[C:6]-[C:7]-[C:8]-1=[O;D1;H0:9]>>[#7:5]-[#7:4]1-[C:6]-[C:7]-[C:8](=[O;D1;H0:9])-[CH2;D2;+0:1]-[C:2]-1=[O;D1;H0:3]
22
[{"value": 22.0, "product": "N1(C(CC(CC1)=O)=O)N1CCCCC1", "details": "PERCENTYIELD", "is_desired": false}]
125
CELSIUS
null
null
Ethyl 2,4-dioxo-1,1′-bipiperidine-3-carboxylate (11.36 g, 42.38 mmol, Example 14) was dissolved in 10% AcOH (200 mL) and heated at reflux 125° C. for 1 h. The cooled reaction was evaporated, and the residue was purified by flash chromatography using a gradient of 9:1 to 1:1 CH2Cl2/acetone, to give the product as a yell...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester
Ketone
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1.C1CC[NH]CC1
HO-
CC(=O)O
125
null
CCOC(=O)C1C(=O)CCN(N2CCCCC2)C1=O>CC(=O)O>O=C1CCN(N2CCCCC2)C(=O)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b78fc203366846e59b80989b96967b76
CC(=O)CNc1ccc(Cl)cc1Cl.O=C1CCN(N2CCCCC2)C(=O)C1>>Cc1cn(-c2ccc(Cl)cc2Cl)c2c1C(=O)N(N1CCCCC1)CC2
C1(=CC=C(C=C1)S(=O)(=O)O)C.C1(=CC=C(C=C1)S(=O)(=O)O)C.N1(C(CC(CC1)=O)=O)N1CCCCC1.ClC1=C(C=CC(=C1)Cl)NCC(=O)C>>ClC1=C(C=CC(=C1)Cl)N1C=C(C=2C(N(CCC21)N2CCCCC2)=O)C
O=[C:2]([CH3:1])[CH2:3][NH:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[cH:10][c:11]1[Cl:12].O=[C:13]1[CH2:14][C:15](=[O:16])[N:17]([N:18]2[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]2)[CH2:24][CH2:25]1>>[CH3:1][c:2]1[cH:3][n:4](-[c:5]2[cH:6][cH:7][c:8]([Cl:9])[cH:10][c:11]2[Cl:12])[c:13]2[c:14]1[C:15](=[O:16])[N:17]([N:18]1[CH2:19][...
CC(=O)CNc1ccc(Cl)cc1Cl.O=C1CCN(N2CCCCC2)C(=O)C1
Cc1cn(-c2ccc(Cl)cc2Cl)c2c1C(=O)N(N1CCCCC1)CC2
null
null
C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
c3eeaef71a5742d406a57fc1362a058d3239e8e2c1e614ea52e9a298a04273d2
4da15b4213f2884bf2fed954aed7c82e569801281a475847c3bea8d7588b2599
O=C1c2ccn(-c3ccccc3)c2CCN1N1CCCCC1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH2;D2;+0:3]-[NH;D2;+0:4]-[c;H0;D3;+0:5](:[c:6]:[c:7]):[c:8](-[Cl;D1;H0:9]):[c:10].O=[C;H0;D3;+0:11]1-[C:12]-[C:13]-[#7:14](-[#7:15])-[C:16](=[O;D1;H0:17])-[CH2;D2;+0:18]-1>>[#7:15]-[#7:14]1-[C:13]-[C:12]-[c;H0;D3;+0:11]2:[c;H0;D3;+0:18](:[c;H0;D3;+0:1](-[C;D1;H3:2]):[cH;D2;+0:3]:[n;H0;D...
43
[{"value": 43.0, "product": "ClC1=C(C=CC(=C1)Cl)N1C=C(C=2C(N(CCC21)N2CCCCC2)=O)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 1,1′-bipiperidine-2,4-dione (Example 15) (260 mg, 1.32 mmol) in dry toluene (25 mL) at rt were added 1-[(2,4-dichlorophenyl)amino]acetone (288 mg, 1.32 mmol, prepared in a similar manner to Example 25) followed by p-TSA (p-toluenesulfonic acid) (25 mg, 0.132 mmol). The mixture was heated at reflux with...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone.Secondary amine
null
C1CC[NH]CC1
C1NCCc2[nH]ccc21
c1ccccc1.C1NCCc2[nH]ccc21.C1CC[NH]CC1
HO-
C1(=CC=CC=C1)C
null
null
CC(=O)CNc1ccc(Cl)cc1Cl.O=C1CCN(N2CCCCC2)C(=O)C1>C1(=CC=CC=C1)C>Cc1cn(-c2ccc(Cl)cc2Cl)c2c1C(=O)N(N1CCCCC1)CC2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fc4081945ad94a06b2047b2452355331
Cc1cn(-c2ccc(Cl)cc2Cl)c2c1C(=O)N(N1CCCCC1)CC2.O=C1CCC(=O)N1Br>>Cc1c2c(n(-c3ccc(Cl)cc3Cl)c1Br)CCN(N1CCCCC1)C2=O
O.ClC1=C(C=CC(=C1)Cl)N1C=C(C=2C(N(CCC21)N2CCCCC2)=O)C.BrN1C(CCC1=O)=O>>BrC1=C(C=2C(N(CCC2N1C1=C(C=C(C=C1)Cl)Cl)N1CCCCC1)=O)C
[CH3:1][c:2]1[c:3]2[c:4]([n:5](-[c:6]3[cH:7][cH:8][c:9]([Cl:10])[cH:11][c:12]3[Cl:13])[cH:14]1)[CH2:16][CH2:17][N:18]([N:19]1[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24]1)[C:25]2=[O:26].O=C1CCC(=O)N1[Br:15]>>[CH3:1][c:2]1[c:3]2[c:4]([n:5](-[c:6]3[cH:7][cH:8][c:9]([Cl:10])[cH:11][c:12]3[Cl:13])[c:14]1[Br:15])[CH2:16][CH2:17...
Cc1cn(-c2ccc(Cl)cc2Cl)c2c1C(=O)N(N1CCCCC1)CC2.O=C1CCC(=O)N1Br
Cc1c2c(n(-c3ccc(Cl)cc3Cl)c1Br)CCN(N1CCCCC1)C2=O
null
null
CN(C)C=O
Functional Group Interconversion
Bromination
0d9e251feb1fbae287306eec2368c8454cdb94b72683e437e8d7c15e30126037
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
O=C1c2ccn(-c3ccccc3)c2CCN1N1CCCCC1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[#7:2]-[C:3](=[O;D1;H0:4])-[c:5]1:[c:6]:[#7;a:7](-[c:8]):[cH;D2;+0:9]:[c:10]:1-[C;D1;H3:11]>>[#7:2]-[C:3](=[O;D1;H0:4])-[c:5]1:[c:6]:[#7;a:7](-[c:8]):[c;H0;D3;+0:9](-[Br;H0;D1;+0:1]):[c:10]:1-[C;D1;H3:11]
75
[{"value": 75.0, "product": "BrC1=C(C=2C(N(CCC2N1C1=C(C=C(C=C1)Cl)Cl)N1CCCCC1)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 74.4, "product": "BrC1=C(C=2C(N(CCC2N1C1=C(C=C(C=C1)Cl)Cl)N1CCCCC1)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
To a solution of 1-(2,4-dichlorophenyl)-3-methyl-5-(1-piperidinyl)-1,5,6,7-tetrahydro-4H-pyrrolo[3,2-c]pyridin-4-one (200 mg, 0.529 mmol, Example 16) at 0° C. in dry DMF was added NBS (N-bromosuccinimide) (99 mg, 0.555 mmol). The reaction mixture was stirred 1 h at 0° C., and then water was added. The resulting solutio...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
C1NCCc2[nH]ccc21.C1CCNC1
C1NCCc2[nH]ccc21
c1ccccc1.C1NCCc2[nH]ccc21.C1CC[NH]CC1
HO-
CN(C)C=O
0
1
Cc1cn(-c2ccc(Cl)cc2Cl)c2c1C(=O)N(N1CCCCC1)CC2.O=C1CCC(=O)N1Br>CN(C)C=O>Cc1c2c(n(-c3ccc(Cl)cc3Cl)c1Br)CCN(N1CCCCC1)C2=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9d88810ec3fa46f2b9843685a10f101f
COc1ccc(-c2c(C)c3c(n2-c2ccccc2Cl)CCN([C@H]2CCCC[C@@H]2OCc2ccccc2)C3=O)cc1>>COc1ccc(-c2c(C)c3c(n2-c2ccccc2Cl)CCN([C@H]2CCCC[C@@H]2O)C3=O)cc1
C(C1=CC=CC=C1)O[C@@H]1[C@H](CCCC1)N1C(C2=C(CC1)N(C(=C2C)C2=CC=C(C=C2)OC)C2=C(C=CC=C2)Cl)=O.C(C1=CC=CC=C1)O[C@@H]1[C@H](CCCC1)N.C(C1=CC=CC=C1)O[C@@H]1[C@H](CCCC1)N1C(C2=C(CC1)N(C(=C2C)C2=CC=C(C=C2)OC)C2=C(C=CC=C2)Cl)=O.C[Si](C)(C)I.ClC1=C(C=CC=C1)N1C(=CC=2CNCCC21)C2=CC=C(C=C2)OC>>ClC1=C(C=CC=C1)N1C(=C(C=2C(N(CCC21)[C@@H...
c1ccc(C[O:29][C@@H:28]2[C@@H:23]([N:22]3[CH2:21][CH2:20][c:11]4[c:10]([c:8]([CH3:9])[c:7](-[c:6]5[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:33][cH:32]5)[n:12]4-[c:13]4[cH:14][cH:15][cH:16][cH:17][c:18]4[Cl:19])[C:30]3=[O:31])[CH2:24][CH2:25][CH2:26][CH2:27]2)cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[c:8]([CH3:9])[c:10]3...
COc1ccc(-c2c(C)c3c(n2-c2ccccc2Cl)CCN([C@H]2CCCC[C@@H]2OCc2ccccc2)C3=O)cc1
COc1ccc(-c2c(C)c3c(n2-c2ccccc2Cl)CCN([C@H]2CCCC[C@@H]2O)C3=O)cc1
null
null
C(Cl)Cl
Deprotection
Hydroxyl benzyl deprotection
655dc7217e93a347240a9b37b98ac62a0e37873ad7f15572a101946745db77a8
32e9a9ca3191eb6608eee26da72fef0d2c2afd087eefdbcc65ce4c46772064f8
O=C1c2cc(-c3ccccc3)n(-c3ccccc3)c2CCN1C1CCCCC1
[C:1]-[C:2](-[O;H0;D2;+0:3]-C-c1:c:c:c:c:c:1)-[C:4]>>[C:1]-[C:2](-[OH;D1;+0:3])-[C:4]
24
[{"value": 24.0, "product": "ClC1=C(C=CC=C1)N1C(=C(C=2C(N(CCC21)[C@@H]2[C@H](CCCC2)O)=O)C)C2=CC=C(C=C2)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
The starting material for this example, namely 5-[(1S,2S)-2-(benzyloxy)cyclohexyl]-1-(2-chlorophenyl)-2-(4-methoxyphenyl)-3-methyl-1,5,6,7-tetrahydro-4H-pyrrolo[3,2-c]pyridin-4-one, was prepared by following the methods described in Scheme 2 and Examples 12–19, using (1S,2S)-2-(benzyloxy)cyclohexylamine as R4NH2 (Schem...
10.6084/m9.figshare.5104873.v1
null
Ether
Secondary alcohol
c1ccccc1
null
c1ccccc1.c1ccccc1.C1NCCc2[nH]ccc21.C1CCCCC1
Other
C(Cl)Cl
null
18
COc1ccc(-c2c(C)c3c(n2-c2ccccc2Cl)CCN([C@H]2CCCC[C@@H]2OCc2ccccc2)C3=O)cc1>C(Cl)Cl>COc1ccc(-c2c(C)c3c(n2-c2ccccc2Cl)CCN([C@H]2CCCC[C@@H]2O)C3=O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2ffbd025e5a443f88cec01ba25c5378e
COc1ccc(CN2CCc3c(c(C)c(-c4ccc(Cl)cc4)n3-c3ccc(Cl)cc3Cl)C2=O)c(OC)c1>>Cc1c2c(n(-c3ccc(Cl)cc3Cl)c1-c1ccc(Cl)cc1)CCNC2=O
ClC1=CC=C(C=C1)C1=C(C=2C(N(CCC2N1C1=C(C=C(C=C1)Cl)Cl)CC1=C(C=C(C=C1)OC)OC)=O)C>>ClC1=CC=C(C=C1)C1=C(C=2C(NCCC2N1C1=C(C=C(C=C1)Cl)Cl)=O)C
COc1ccc(C[N:24]2[CH2:23][CH2:22][c:4]3[c:3]([c:2]([CH3:1])[c:14](-[c:15]4[cH:16][cH:17][c:18]([Cl:19])[cH:20][cH:21]4)[n:5]3-[c:6]3[cH:7][cH:8][c:9]([Cl:10])[cH:11][c:12]3[Cl:13])[C:25]2=[O:26])c(OC)c1>>[CH3:1][c:2]1[c:3]2[c:4]([n:5](-[c:6]3[cH:7][cH:8][c:9]([Cl:10])[cH:11][c:12]3[Cl:13])[c:14]1-[c:15]1[cH:16][cH:17][c...
COc1ccc(CN2CCc3c(c(C)c(-c4ccc(Cl)cc4)n3-c3ccc(Cl)cc3Cl)C2=O)c(OC)c1
Cc1c2c(n(-c3ccc(Cl)cc3Cl)c1-c1ccc(Cl)cc1)CCNC2=O
null
null
FC(C(=O)O)(F)F
Reduction
Hydrogenolysis of tertiary amines
83a899b8b971c7ca34e32d1ca65fd04f5e162ee243eccab6230c9b26771e4370
3efc6c7204ad36a2aa7236338bd7163bfb62d1e33efaad6b000b17910587541b
O=C1NCCc2c1cc(-c1ccccc1)n2-c1ccccc1
C-O-c1:c:c:c(-C-[N;H0;D3;+0:1]2-[C:2]-[C:3]-[c:4](:[#7;a:5]):[c:6]-[C:7]-2=[O;D1;H0:8]):c(-O-C):c:1>>[#7;a:5]:[c:4]1:[c:6]-[C:7](=[O;D1;H0:8])-[NH;D2;+0:1]-[C:2]-[C:3]-1
73
[{"value": 73.0, "product": "ClC1=CC=C(C=C1)C1=C(C=2C(NCCC2N1C1=C(C=C(C=C1)Cl)Cl)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.9, "product": "ClC1=CC=C(C=C1)C1=C(C=2C(NCCC2N1C1=C(C=C(C=C1)Cl)Cl)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 2-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-5-(2,4-dimethoxybenzyl)-3-methyl-1,5,6,7-tetrahydro-4H-pyrrolo[3,2-c]pyridin-4-one (1.13 g, 2.03 mmol, Table 2, entry 176) in trifluoroacetic acid (40 mL) was heated at reflux temperature for 2 h. Trifluoroacetic acid was removed by evaporation under reduced press...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Tertiary amide
Secondary amide
c1ccccc1.C1NCCc2nccc21
C1NCCc2[nH]ccc21
c1ccccc1.c1ccccc1.C1NCCc2[nH]ccc21
HO-
FC(C(=O)O)(F)F
null
null
COc1ccc(CN2CCc3c(c(C)c(-c4ccc(Cl)cc4)n3-c3ccc(Cl)cc3Cl)C2=O)c(OC)c1>FC(C(=O)O)(F)F>Cc1c2c(n(-c3ccc(Cl)cc3Cl)c1-c1ccc(Cl)cc1)CCNC2=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5ee44bbe9ff84184b47548d3f878aee1
CC(=O)CI.Nc1ccccc1Cl>>CC(=O)CNc1ccccc1Cl
ClC1=C(N)C=CC=C1.ICC(C)=O.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>>ClC1=C(C=CC=C1)NCC(=O)C
I[CH2:4][C:2]([CH3:1])=[O:3].[NH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][c:11]1[Cl:12]>>[CH3:1][C:2](=[O:3])[CH2:4][NH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][c:11]1[Cl:12]
CC(=O)CI.Nc1ccccc1Cl
CC(=O)CNc1ccccc1Cl
null
null
O
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
c176e63a024701466caae2c04d3f5d2104f6d3bb155f520591ae3ee416bc3e3e
aa31def40a661a269b8a0fab7756768062834fd7bfb5c5af11ba9793df9868ba
c1ccccc1
I-[CH2;D2;+0:1]-[C:2](-[C;D1;H3:3])=[O;D1;H0:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[C;D1;H3:3]-[C:2](=[O;D1;H0:4])-[CH2;D2;+0:1]-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]
90.1
[{"value": 77.0, "product": "ClC1=C(C=CC=C1)NCC(=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.1, "product": "ClC1=C(C=CC=C1)NCC(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of chloroacetone (8.0 mL, 0.100 mol) in 100 mL acetone was added KI (33.20 g, 0.200 mol). The suspension was stirred under argon at rt for 24 h. Acetone was evaporated under reduced pressure. The residue was extracted with ether. The ethereal solution was concentrated under reduced pressure to yield iodoa...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Primary amine
Ketone.Secondary amine
null
null
c1ccccc1
HI
O
null
null
CC(=O)CI.Nc1ccccc1Cl>O>CC(=O)CNc1ccccc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-25102b621b5e4d25a5e2652806a36518
NO.O=Cc1ccn(-c2ccccc2O)c1>>N#Cc1ccn(-c2ccccc2O)c1
C(=O)C1=CN(C=C1)C1=C(C=CC=C1)O.C(C)N(CC)CC.Cl.NO>>C(#N)C1=CN(C=C1)C1=C(C=CC=C1)O
O[NH2:1].O=[CH:2][c:3]1[cH:4][cH:5][n:6](-[c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[OH:13])[cH:14]1>>[N:1]#[C:2][c:3]1[cH:4][cH:5][n:6](-[c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[OH:13])[cH:14]1
NO.O=Cc1ccn(-c2ccccc2O)c1
N#Cc1ccn(-c2ccccc2O)c1
null
null
C(C)(=O)OC(C)=O
Miscellaneous
OtherReaction
748a00525e7f639e600a6b1229bb8ce947b6e2e96d815c0b05b54470e6cdbc2a
a27285857ea2428fb666a281ae1a2b961eec077cb33a106e48534c99bfe3d865
c1ccc(-n2cccc2)cc1
O-[NH2;D1;+0:1].O=[CH;D2;+0:2]-[c:3]1:[c:4]:[#7;a:5](-[c:6]):[c:7]:[c:8]:1>>[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3]1:[c:4]:[#7;a:5](-[c:6]):[c:7]:[c:8]:1
92
[{"value": 92.0, "product": "C(#N)C1=CN(C=C1)C1=C(C=CC=C1)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 81.4, "product": "C(#N)C1=CN(C=C1)C1=C(C=CC=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
2-(3-Formyl-1-pyrrolyl)phenol (3 g, 16 mmol) and triethylamine (17.6 mmol) are added to a suspension of hydroxylamine hydrochloride (1.22 g, 17.6 mmol) in acetic anhydride (7.7 ml), and the mixture is allowed to stir overnight at ambient temperature. The mixture is refluxed for 5 hours, concentrated, dissolved in 50 ml...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine
Nitrile
null
null
c1cc[nH]c1.c1ccccc1
HO-
C(C)(=O)OC(C)=O
null
8
NO.O=Cc1ccn(-c2ccccc2O)c1>C(C)(=O)OC(C)=O>N#Cc1ccn(-c2ccccc2O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0cf57611eb694aa89dccdcbfac107543
COc1ccccc1B(O)O.N#Cc1ccc(Br)s1>>COc1ccccc1-c1ccc(C#N)s1
ClCCl.BrC1=CC=C(S1)C#N.COC1=C(C=CC=C1)B(O)O.C([O-])([O-])=O.[Na+].[Na+]>>C(#N)C1=CC=C(S1)C1=C(C=CC=C1)OC
OB(O)[c:8]1[c:3]([O:2][CH3:1])[cH:4][cH:5][cH:6][cH:7]1.Br[c:9]1[cH:10][cH:11][c:12]([C:13]#[N:14])[s:15]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1-[c:9]1[cH:10][cH:11][c:12]([C:13]#[N:14])[s:15]1
COc1ccccc1B(O)O.N#Cc1ccc(Br)s1
COc1ccccc1-c1ccc(C#N)s1
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
O1CCOCC1.O
C-C Coupling
Suzuki coupling with boronic acids
a9e750b5cb26673fc488a731642519fa5963d6a2e4d2eeb976470c7f17606def
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cccs2)cc1
Br-[c;H0;D3;+0:1]1:[#16;a:2]:[c:3]:[c:4]:[c:5]:1.O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](-[#8:10]):[c:11]>>[#8:10]-[c:9](:[c:11]):[c;H0;D3;+0:6](-[c;H0;D3;+0:1]1:[#16;a:2]:[c:3]:[c:4]:[c:5]:1):[c:7]:[c:8]
96
[{"value": 96.0, "product": "C(#N)C1=CC=C(S1)C1=C(C=CC=C1)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.7, "product": "C(#N)C1=CC=C(S1)C1=C(C=CC=C1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
A solution of 5-bromothiophene-2-carbonitrile (1.25 g, 6.65 mmol) in 50 ml of dioxane is degassed with argon, tetrakis(triphenylphosphine)palladium(0) (768 mg, 0.665 mmol) is added and the mixture is stirred for 5 minutes. 2-Methoxybenzene boronic acid (2.02 g, 13.3 mmol) and aqueous 2 N sodium carbonate (13.3 ml) are ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
HBr.B
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.O1CCOCC1.O
null
0.083333
COc1ccccc1B(O)O.N#Cc1ccc(Br)s1>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.O1CCOCC1.O>COc1ccccc1-c1ccc(C#N)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-03251ddc1f3e4d94aef166f6ac65dfbe
C=CC(C)=O.Nc1ccccn1.O=C1NC(=O)c2ccccc21>>O=C1c2ccccc2C(=O)N1CCc1cn2ccccc2n1
C=CC(C)=O.C1(C=2C(C(N1)=O)=CC=CC2)=O.BrCC(CCN1C(C2=CC=CC=C2C1=O)=O)=O.NC1=NC=CC=C1>>BrCC(CCN1C(C2=CC=CC=C2C1=O)=O)=O.N=1C(=CN2C1C=CC=C2)CCN2C(C1=CC=CC=C1C2=O)=O
O=[C:31]([CH:30]=[CH2:29])[CH3:32].[n:33]1[cH:34][cH:35][cH:36][cH:37][c:38]1[NH2:39].[O:18]=[C:19]1[c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]2[C:26](=[O:27])[NH:28]1>>[O:18]=[C:19]1[c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]2[C:26](=[O:27])[N:28]1[CH2:29][CH2:30][c:31]1[cH:32][n:33]2[cH:34][cH:35][cH:36][cH:37][c:38]2[n:...
C=CC(C)=O.Nc1ccccn1.O=C1NC(=O)c2ccccc21
O=C1c2ccccc2C(=O)N1CCc1cn2ccccc2n1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
fe19272faa31f0cb9f07f60ebae4a5d6da5396213b603a1c83271580797fbf6e
bad28b42d078f16f7e7f6d5fbd1d95e2bb8a5073fbdb3d319b6480dc943a901f
O=C1c2ccccc2C(=O)N1CCc1cn2ccccc2n1
O=[C;H0;D3;+0:1](-[CH3;D1;+0:2])-[CH;D2;+0:3]=[CH2;D1;+0:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[n;H0;D2;+0:8]:[c:9]:[c:10].[O;D1;H0:11]=[C:12]1-[NH;D2;+0:13]-[C:14](=[O;D1;H0:15])-[c:16]:[c:17]-1>>[O;D1;H0:11]=[C:12]1-[c:17]:[c:16]-[C:14](=[O;D1;H0:15])-[N;H0;D3;+0:13]-1-[CH2;D2;+0:4]-[CH2;D2;+0:3]-[c;H0;D3;+0:1]1:[cH;D2;+0:2...
96.6
[{"value": 49.0, "product": "N=1C(=CN2C1C=CC=C2)CCN2C(C1=CC=CC=C1C2=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.6, "product": "N=1C(=CN2C1C=CC=C2)CCN2C(C1=CC=CC=C1C2=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-(4-Bromo-3-oxo-butyl)-isoindole-1,3-dione is prepared by condensation of but-1-en-3-one with phthalimide followed by bromination according to known procedures (J. Med. Chem., 35:3239, 1992. A solution of 2-(4-bromo-3-oxo-butyl)-isoindole-1,3-dione (8.9 g, 30.06 mmol) and 2-aminopyridine (2.8 g, 29.75 mmol) in ethanol...
10.6084/m9.figshare.5104873.v1
null
Ketone.Unsubstituted dicarboximide.Primary amine.Vinyl
Substituted dicarboximide
c1ccncc1.c1ccc2c(c1)CNC2
c1ccc2c(c1)C[NH]C2.c1ccn2ccnc2c1
c1ccc2c(c1)C[NH]C2.c1ccn2ccnc2c1
HO-
C(C)O
null
null
C=CC(C)=O.Nc1ccccn1.O=C1NC(=O)c2ccccc21>C(C)O>O=C1c2ccccc2C(=O)N1CCc1cn2ccccc2n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-37ed76e448754df0a9ef4d3a2cb23443
CC(C)(N)CC(=O)O.O=C1OC(=O)c2ccccc21>>CC(C)(CC(=O)O)N1C(=O)c2ccccc2C1=O
NC(CC(=O)O)(C)C.C1(C=2C(C(=O)O1)=CC=CC2)=O>>CC(CC(=O)O)(N1C(C2=CC=CC=C2C1=O)=O)C
[CH3:1][C:2]([CH3:3])([CH2:4][C:5](=[O:6])[OH:7])[NH2:8].O1[C:9](=[O:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[C:17]1=[O:18]>>[CH3:1][C:2]([CH3:3])([CH2:4][C:5](=[O:6])[OH:7])[N:8]1[C:9](=[O:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[C:17]1=[O:18]
CC(C)(N)CC(=O)O.O=C1OC(=O)c2ccccc21
CC(C)(CC(=O)O)N1C(=O)c2ccccc2C1=O
null
null
C(C)O
Acylation
Phthalic anhydride to phthalimide
c3c986d6e09320348d40a4a59ca107882ce771f249842049dc55e55f334c675b
2bbbf7b24648445e31d33a2a26f8618c2067bd23957587cc459f3c45a03ed48a
O=C1NC(=O)c2ccccc21
[C;D1;H3:1]-[C:2](-[C;D1;H3:3])(-[NH2;D1;+0:4])-[C:5]-[C:6](=[O;D1;H0:7])-[O;D1;H1:8].[O;D1;H0:9]=[C;H0;D3;+0:10]1-O-[C;H0;D3;+0:11](=[O;D1;H0:12])-[c:13](:[c:14]):[c:15]-1:[c:16]>>[C;D1;H3:1]-[C:2](-[C;D1;H3:3])(-[C:5]-[C:6](=[O;D1;H0:7])-[O;D1;H1:8])-[N;H0;D3;+0:4]1-[C;H0;D3;+0:11](=[O;D1;H0:12])-[c:13](:[c:14]):[c:1...
58
[{"value": 58.0, "product": "CC(CC(=O)O)(N1C(C2=CC=CC=C2C1=O)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 33.2, "product": "CC(CC(=O)O)(N1C(C2=CC=CC=C2C1=O)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
180
CELSIUS
54
HOUR
An intimate mixture of of 3-amino-3-methyl butanoic acid (27.4 g, 0.234 mol) and phthalic anhydride (38.1 g, 0.257 mol) is heated at 180° C. for 1.5 hours. After cooling, the reaction mixture is dissolved in 40 ml of ethanol and kept in a refrigerator for 54 hours. The colorless crystalline precipitate thus obtained is...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Ester.Ester.Primary amine
Substituted dicarboximide
c1ccc2c(c1)COC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2
HO-
C(C)O
180
54
CC(C)(N)CC(=O)O.O=C1OC(=O)c2ccccc21>C(C)O>CC(C)(CC(=O)O)N1C(=O)c2ccccc2C1=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b797af70be854695acaa06e83a90aaeb
CC(C)(CC(=O)O)N1C(=O)c2ccccc2C1=O.NCc1ccccn1>>CC(C)(CC(=O)NCc1ccccn1)N1C(=O)c2ccccc2C1=O
CC(CC(=O)O)(N1C(C2=CC=CC=C2C1=O)=O)C.NCC1=NC=CC=C1>>N1=C(C=CC=C1)CNC(CC(N1C(C2=CC=CC=C2C1=O)=O)(C)C)=O
O[C:5]([CH2:4][C:2]([CH3:1])([CH3:3])[N:15]1[C:16](=[O:17])[c:18]2[cH:19][cH:20][cH:21][cH:22][c:23]2[C:24]1=[O:25])=[O:6].[NH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][n:14]1>>[CH3:1][C:2]([CH3:3])([CH2:4][C:5](=[O:6])[NH:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][n:14]1)[N:15]1[C:16](=[O:17])[c:18]2[cH:19][cH:20]...
CC(C)(CC(=O)O)N1C(=O)c2ccccc2C1=O.NCc1ccccn1
CC(C)(CC(=O)NCc1ccccn1)N1C(=O)c2ccccc2C1=O
null
null
C(Cl)Cl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(CCN1C(=O)c2ccccc2C1=O)NCc1ccccn1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[#7;a:5]:[c:6]-[C:7]-[NH2;D1;+0:8]>>[#7;a:5]:[c:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]
58.3
[{"value": 58.0, "product": "N1=C(C=CC=C1)CNC(CC(N1C(C2=CC=CC=C2C1=O)=O)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 58.3, "product": "N1=C(C=CC=C1)CNC(CC(N1C(C2=CC=CC=C2C1=O)=O)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
To a solution of β,β-dimethyl-1,3-dioxo-2-isoindolinepropionic acid (5 g, 20.2 mmol) and N,N-dicyclohexylcarbodiimide (4.6 g, 22.24 mmol) in 50 ml of dry methylene chloride is added 2-(aminomethyl)pyridine (2.41 g, 2.3 ml, 22.24 mmol) at ambient temperature. The mixture is stirred for 24 hours. The precipitate of dicyc...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccncc1.c1ccc2c(c1)C[NH]C2
HO-
C(Cl)Cl
null
24
CC(C)(CC(=O)O)N1C(=O)c2ccccc2C1=O.NCc1ccccn1>C(Cl)Cl>CC(C)(CC(=O)NCc1ccccn1)N1C(=O)c2ccccc2C1=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-735b516f55264b85ba2e9e18846ec391
C=[N+](C)C.[I-].c1cnc2[nH]ccc2c1>>CN(C)Cc1c[nH]c2ncccc12.I
N1C=CC2=CC=CN=C12.C[N+](=C)C.[I-]>>I.CN(C)CC1=CNC2=NC=CC=C12
[CH3:1][N+:2]([CH3:3])=[CH2:4].[I-:14].[cH:5]1[cH:6][nH:7][c:8]2[n:9][cH:10][cH:11][cH:12][c:13]12>>[CH3:1][N:2]([CH3:3])[CH2:4][c:5]1[cH:6][nH:7][c:8]2[n:9][cH:10][cH:11][cH:12][c:13]12.[IH:14]
C=[N+](C)C.[I-].c1cnc2[nH]ccc2c1
CN(C)Cc1c[nH]c2ncccc12.I
null
null
C(C)(=O)O
C-C Coupling
OtherReaction
056025bccbd355e6a7ea9f01f673db1cd68dd717ff514abfa298d9bfd557edfe
5c03404e5740858973798689d4be0a8ed62608f5043e578ba3cd6de4363e2dbe
c1cnc2[nH]ccc2c1
[C;D1;H3:1]-[N+;H0;D3:2](-[C;D1;H3:3])=[CH2;D1;+0:4].[I-;H0;D0:5].[c:6]:[#7;a:7]:[c:8]1:[#7;a:9]:[c:10]:[cH;D2;+0:11]:[c:12]:1:[c:13]>>[C;D1;H3:1]-[N;H0;D3;+0:2](-[C;D1;H3:3])-[CH2;D2;+0:4]-[c;H0;D3;+0:11]1:[c:10]:[#7;a:9]:[c:8](:[#7;a:7]:[c:6]):[c:12]:1:[c:13].[IH;D0;+0:5]
null
[]
65
CELSIUS
null
null
7-Azaindole (5.05 g, 43 mmol) and Eschenmoser's salt (N,N-dimethylmethyleneammonium iodide; 8.48 g, 45 mmol) are combined in 100 ml of glacial acetic acid. After heating at 65° C. for 1 hour, the reaction mixture is concentrated in vacuo. The resulting solid is triturated with ethyl acetate, filtered and dried in vacuo...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amine
c1cnc2[nH]ccc2c1
c1cnc2[nH]ccc2c1
c1cnc2[nH]ccc2c1
null
C(C)(=O)O
65
null
C=[N+](C)C.[I-].c1cnc2[nH]ccc2c1>C(C)(=O)O>CN(C)Cc1c[nH]c2ncccc12.I
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-eea38e3147f941809ffb13454bc8a7c8
CC(C)[N+](=O)[O-].CN(C)Cc1c[nH]c2ncccc12>>CC(C)(Cc1c[nH]c2ncccc12)[N+](=O)[O-]
I.CN(C)CC1=CNC2=NC=CC=C12.CI.C[O-].[Na+].[N+](=O)([O-])C(C)C>>CC(CC1=CNC2=NC=CC=C12)(C)[N+](=O)[O-]
[CH3:1][CH:2]([CH3:3])[N+:14](=[O:15])[O-:16].CN(C)[CH2:4][c:5]1[cH:6][nH:7][c:8]2[n:9][cH:10][cH:11][cH:12][c:13]12>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[n:9][cH:10][cH:11][cH:12][c:13]12)[N+:14](=[O:15])[O-:16]
CC(C)[N+](=O)[O-].CN(C)Cc1c[nH]c2ncccc12
CC(C)(Cc1c[nH]c2ncccc12)[N+](=O)[O-]
null
null
[NH4+].[Cl-].CO.C(C)(=O)OCC
C-C Coupling
OtherReaction
410d0ecf550dfec32b5bd37f61aeafc75533d5e4329aa3110c08acb15e21dcaa
fc73a0ba4f6f90cb21df47612bcde105fcd2a049cd56b52924f944fc6a6cbe55
c1cnc2[nH]ccc2c1
C-N(-C)-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4](:[#7;a:5]):[#7;a:6]:[c:7]:1.[C;D1;H3:8]-[CH;D3;+0:9](-[C;D1;H3:10])-[#7;+:11](-[O;-;D1;H0:12])=[O;D1;H0:13]>>[#7;a:5]:[c:4]1:[#7;a:6]:[c:7]:[c:2](-[CH2;D2;+0:1]-[C;H0;D4;+0:9](-[C;D1;H3:8])(-[C;D1;H3:10])-[#7;+:11](-[O;-;D1;H0:12])=[O;D1;H0:13]):[c:3]:1
92
[{"value": 92.0, "product": "CC(CC1=CNC2=NC=CC=C12)(C)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A 0° C. solution of 3-dimethylaminomethyl-1H-7-azaindole hydroiodide (10 g, 33 mmol) in 46 ml of methanol and 46 ml of 2-nitropropane is treated with methyl iodide (2.15 ml, 35 mmol) and solid sodium methoxide (3.65 g, 68 mmol) sequentially. The resulting mixture is allowed to warm to ambient temperature, and, after st...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Tertiary amine
Nitro group
null
null
c1cnc2[nH]ccc2c1
Other
[NH4+].[Cl-].CO.C(C)(=O)OCC
null
8
CC(C)[N+](=O)[O-].CN(C)Cc1c[nH]c2ncccc12>[NH4+].[Cl-].CO.C(C)(=O)OCC>CC(C)(Cc1c[nH]c2ncccc12)[N+](=O)[O-]
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bcd96f282a0b42aebd3d55cb6b3b5052
BrBr.C=CC=O.CC(C)[N+](=O)[O-]>>CC(C)(CC(Br)C=O)[N+](=O)[O-]
C(=O)C=C.[N+](=O)([O-])C(C)C.CC(CCC=O)(C)[N+](=O)[O-].BrBr>>CC(CCC=O)(C)[N+](=O)[O-].BrC(C=O)CC(C)([N+](=O)[O-])C
Br[Br:6].[CH2:1]=[CH:5][CH:7]=[O:8].[CH:2]([CH3:3])([CH3:4])[N+:9](=[O:10])[O-:11]>>[CH3:1][C:2]([CH3:3])([CH2:4][CH:5]([Br:6])[CH:7]=[O:8])[N+:9](=[O:10])[O-:11]
BrBr.C=CC=O.CC(C)[N+](=O)[O-]
CC(C)(CC(Br)C=O)[N+](=O)[O-]
null
null
O.C(C)(=O)O
C-C Coupling
OtherReaction
bd3ac79662011be9149b4c953fba45a902bf7153fc7cbf85f8297521df255f54
2d5d05895dd6418ad448d0782a091325da1d87ac6d371c11269c83d301868b70
null
Br-[Br;H0;D1;+0:1].[C;D1;H3:2]-[CH;D3;+0:3](-[CH3;D1;+0:4])-[#7;+:5](-[O;-;D1;H0:6])=[O;D1;H0:7].[CH2;D1;+0:8]=[CH;D2;+0:9]-[C:10]=[O;D1;H0:11]>>[Br;H0;D1;+0:1]-[CH;D3;+0:9](-[C:10]=[O;D1;H0:11])-[CH2;D2;+0:4]-[C;H0;D4;+0:3](-[C;D1;H3:2])(-[CH3;D1;+0:8])-[#7;+:5](-[O;-;D1;H0:6])=[O;D1;H0:7]
163.1
[{"value": 163.1, "product": "BrC(C=O)CC(C)([N+](=O)[O-])C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
4-Methyl-4-nitropentanal is prepared by condensation of acrolein and 2-nitropropane according to a known procedure (Synthesis 1986, 237). To a solution of 4-methyl-4-nitropentanal (8.5 g, 58.56 mmol) in acetic acid (125 ml) is added bromine (9.12 g, 57.07 mmol) dropwise while the temperature is kept below 15° C. After ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Nitro group.Vinyl
Secondary halide.Aldehyde.Nitro group
null
null
null
HBr
O.C(C)(=O)O
null
0.25
BrBr.C=CC=O.CC(C)[N+](=O)[O-]>O.C(C)(=O)O>CC(C)(CC(Br)C=O)[N+](=O)[O-]
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8f7b661a8c334a4c812e0988775af118
CC(C)(CC(Br)C=O)[N+](=O)[O-].Nc1ncccc1OCc1ccccc1>>CC(C)(Cc1cnc2c(OCc3ccccc3)cccn12)[N+](=O)[O-]
NC1=NC=CC=C1OCC1=CC=CC=C1.BrC(C=O)CC(C)([N+](=O)[O-])C>>CC(CC1=CN=C2N1C=CC=C2OCC2=CC=CC=C2)(C)[N+](=O)[O-]
O=[CH:6][CH:5](Br)[CH2:4][C:2]([CH3:1])([CH3:3])[N+:22](=[O:23])[O-:24].[NH2:7][c:8]1[c:9]([O:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[cH:18][cH:19][cH:20][n:21]1>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][n:7][c:8]2[c:9]([O:10][CH2:11][c:12]3[cH:13][cH:14][cH:15][cH:16][cH:17]3)[cH:18][cH:19][cH:20][n:2...
CC(C)(CC(Br)C=O)[N+](=O)[O-].Nc1ncccc1OCc1ccccc1
CC(C)(Cc1cnc2c(OCc3ccccc3)cccn12)[N+](=O)[O-]
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
3a7835efa5ac56b87be43234b54606ae621fc957a5ff407573e590f6174c2545
4efe5597cd78b75eedda88a299158b349ae1f03c7cd5a6a1daf8cec0515aae7c
c1ccc(COc2cccn3ccnc23)cc1
Br-[CH;D3;+0:1](-[C:2]-[C:3])-[CH;D2;+0:4]=O.[NH2;D1;+0:5]-[c:6](:[c:7]):[n;H0;D2;+0:8]:[c:9]:[c:10]>>[C:3]-[C:2]-[c;H0;D3;+0:1]1:[cH;D2;+0:4]:[n;H0;D2;+0:5]:[c:6](:[c:7]):[n;H0;D3;+0:8]:1:[c:9]:[c:10]
64.4
[{"value": 64.0, "product": "CC(CC1=CN=C2N1C=CC=C2OCC2=CC=CC=C2)(C)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 64.4, "product": "CC(CC1=CN=C2N1C=CC=C2OCC2=CC=CC=C2)(C)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
A mixture of 2-amino-3-benzyloxypyridine (2.7 g, 13.5 mmol) and 2-bromo-4-methyl-4-nitropentanal (3.0 g, 13.5 mmol) in ethanol (20 ml) is heated at 100° C. overnight. The solvent is removed under reduced pressure and the residue is treated with saturated aqueous NaHCO3 solution. The aqueous mixture is extracted two tim...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Aldehyde.Primary amine
null
c1ccncc1
c1ccn2ccnc2c1
c1ccccc1.c1ccn2ccnc2c1
HBr
C(C)O
100
null
CC(C)(CC(Br)C=O)[N+](=O)[O-].Nc1ncccc1OCc1ccccc1>C(C)O>CC(C)(Cc1cnc2c(OCc3ccccc3)cccn12)[N+](=O)[O-]
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6acc8a33ef804c1a86c2573a8963d318
CC(C)(Cc1cnc2cc(O)ccn12)[N+](=O)[O-].NC(=O)CCl>>CC(C)(Cc1cnc2cc(OCC(N)=O)ccn12)[N+](=O)[O-]
CC(CC1=CN=C2N1C=CC(=C2)O)(C)[N+](=O)[O-].ClCC(=O)N.C([O-])([O-])=O.[K+].[K+].[I-].[K+]>>CC(CC1=CN=C2N1C=CC(=C2)OCC(=O)N)(C)[N+](=O)[O-]
[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][n:7][c:8]2[cH:9][c:10]([OH:11])[cH:16][cH:17][n:18]12)[N+:19](=[O:20])[O-:21].Cl[CH2:12][C:13]([NH2:14])=[O:15]>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][n:7][c:8]2[cH:9][c:10]([O:11][CH2:12][C:13]([NH2:14])=[O:15])[cH:16][cH:17][n:18]12)[N+:19](=[O:20])[O-:21]
CC(C)(Cc1cnc2cc(O)ccn12)[N+](=O)[O-].NC(=O)CCl
CC(C)(Cc1cnc2cc(OCC(N)=O)ccn12)[N+](=O)[O-]
null
null
CC(CC)=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccn2ccnc2c1
Cl-[CH2;D2;+0:1]-[C:2](-[N;D1;H2:3])=[O;D1;H0:4].[#7;a:5]:[c:6]1:[#7;a:7]:[c:8]:[c:9]:[c:10](-[OH;D1;+0:11]):[c:12]:1>>[#7;a:5]:[c:6]1:[#7;a:7]:[c:8]:[c:9]:[c:10](-[O;H0;D2;+0:11]-[CH2;D2;+0:1]-[C:2](-[N;D1;H2:3])=[O;D1;H0:4]):[c:12]:1
34.3
[{"value": 34.0, "product": "CC(CC1=CN=C2N1C=CC(=C2)OCC(=O)N)(C)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 34.3, "product": "CC(CC1=CN=C2N1C=CC(=C2)OCC(=O)N)(C)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
3-(2-Methyl-2-nitropropyl)imidazo[1,2-a]pyridin-7-ol (1.5 g, 6.38 mmol), chloroacetamide (1.19 g, 12.73 mmol), potassium carbonate (6.4 mmol) and a small amount of potassium iodide in 2-butanone (30 ml) is heated at reflux overnight. The solids are removed by filtration and the filtrate is concentrated under reduced pr...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccn2ccnc2c1
HCl
CC(CC)=O
null
null
CC(C)(Cc1cnc2cc(O)ccn12)[N+](=O)[O-].NC(=O)CCl>CC(CC)=O>CC(C)(Cc1cnc2cc(OCC(N)=O)ccn12)[N+](=O)[O-]
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a7d971e9763c4e23bba9f02f13b16231
CC(C)(CC(Br)C=O)[N+](=O)[O-].Cc1ccnc(N)c1>>Cc1ccn2c(CC(C)(C)[N+](=O)[O-])cnc2c1
NC1=NC=CC(=C1)C.BrC(C=O)CC(C)([N+](=O)[O-])C>>CC1=CC=2N(C=C1)C(=CN2)CC(C)([N+](=O)[O-])C
O=[CH:14][CH:6](Br)[CH2:7][C:8]([CH3:9])([CH3:10])[N+:11](=[O:12])[O-:13].[CH3:1][c:2]1[cH:3][cH:4][n:5][c:16]([NH2:15])[cH:17]1>>[CH3:1][c:2]1[cH:3][cH:4][n:5]2[c:6]([CH2:7][C:8]([CH3:9])([CH3:10])[N+:11](=[O:12])[O-:13])[cH:14][n:15][c:16]2[cH:17]1
CC(C)(CC(Br)C=O)[N+](=O)[O-].Cc1ccnc(N)c1
Cc1ccn2c(CC(C)(C)[N+](=O)[O-])cnc2c1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
3a7835efa5ac56b87be43234b54606ae621fc957a5ff407573e590f6174c2545
4efe5597cd78b75eedda88a299158b349ae1f03c7cd5a6a1daf8cec0515aae7c
c1ccn2ccnc2c1
Br-[CH;D3;+0:1](-[C:2]-[C:3])-[CH;D2;+0:4]=O.[NH2;D1;+0:5]-[c:6](:[c:7]):[n;H0;D2;+0:8]:[c:9]:[c:10]>>[C:3]-[C:2]-[c;H0;D3;+0:1]1:[cH;D2;+0:4]:[n;H0;D2;+0:5]:[c:6](:[c:7]):[n;H0;D3;+0:8]:1:[c:9]:[c:10]
63.4
[{"value": 63.0, "product": "CC1=CC=2N(C=C1)C(=CN2)CC(C)([N+](=O)[O-])C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 63.4, "product": "CC1=CC=2N(C=C1)C(=CN2)CC(C)([N+](=O)[O-])C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Amino-4-methylpyridine (2.2 g, 20.3 mmol) and 2-bromo-4-methyl4-nitropentanal (20.3 mmol) are reacted as described in Amine 7 to give 3.0 g of 7-methyl-3-(2-methyl-2-nitropropyl)imidazo[1,2-a]pyridine (63%). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Aldehyde.Primary amine
null
c1ccncc1
c1ccn2ccnc2c1
c1ccn2ccnc2c1
HBr
null
null
null
CC(C)(CC(Br)C=O)[N+](=O)[O-].Cc1ccnc(N)c1>>Cc1ccn2c(CC(C)(C)[N+](=O)[O-])cnc2c1