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-c34472859da14a81bfe0f74e60f15c43
ord-999349dc79214221aaf430c3096dbad1
Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1.[N-]=C=O>>NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
[N-]=C=O.[K+].FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1.[N-]=C=O.[K+].O.C([O-])(O)=O.[Na+]>>FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(=O)N
[NH:4]1[CH2:5][CH2:6][S:7][CH:8]1[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[O:15][CH2:16][CH2:17][N:18]1[CH2:19][CH2:20][N:21]([c:22]2[cH:23][cH:24][cH:25][c:26]([F:27])[cH:28]2)[CH2:29][CH2:30]1.[N-:1]=[C:2]=[O:3]>>[NH2:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][S:7][CH:8]1[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[O:15][CH2:1...
Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1.[N-]=C=O
NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
C(C)(=O)O.C(C)O
Acylation
OtherReaction
19b1a78eac5c11a7a6d62add8e898dd94b39712d8c09ceabf81d7e8d852d9904
c12a5f5aa1bd3b17571900882f538b1b74958bac9a5fa2923f5c850cbafbf1dd
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
[N-;H0;D1:1]=[C;H0;D2;+0:2]=[O;D1;H0:3].[c:4]-[C:5]1-[#16:6]-[C:7]-[C:8]-[NH;D2;+0:9]-1>>[NH2;D1;+0:1]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[N;H0;D3;+0:9]1-[C:8]-[C:7]-[#16:6]-[C:5]-1-[c:4]
87.3
[{"value": 87.3, "product": "FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(=O)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A mixture of 1.12 g of potassium isocyanate, 10 ml of water and 2 ml of acetic acid is added to a solution of 2.68 g of 2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine in 20 ml of ethanol, and the mixture is stirred at room temperature for 2 hours. A mixture of 0.56 g of potassium isocyanate and ...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Urea
C1CSCN1
C1CSC[NH]1
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
null
C(C)(=O)O.C(C)O
null
2
Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1.[N-]=C=O>C(C)(=O)O.C(C)O>NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-99a875cbc0914ffc94f639c96f95744e
[N-]=C=O.c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1>>NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
[N-]=C=O.[Na+].C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1.C(C)(=O)O.C([O-])([O-])=O.[K+].[K+]>>C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(=O)N
[N-:1]=[C:2]=[O:3].[NH:4]1[CH2:5][CH2:6][S:7][CH:8]1[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[O:15][CH2:16][CH2:17][N:18]1[CH2:19][CH2:20][N:21]([c:22]2[cH:23][cH:24][cH:25][cH:26][cH:27]2)[CH2:28][CH2:29]1>>[NH2:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][S:7][CH:8]1[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[O:15][CH2:16][CH2:...
[N-]=C=O.c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
null
null
O.C(C)O
Acylation
OtherReaction
19b1a78eac5c11a7a6d62add8e898dd94b39712d8c09ceabf81d7e8d852d9904
c12a5f5aa1bd3b17571900882f538b1b74958bac9a5fa2923f5c850cbafbf1dd
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
[N-;H0;D1:1]=[C;H0;D2;+0:2]=[O;D1;H0:3].[c:4]-[C:5]1-[#16:6]-[C:7]-[C:8]-[NH;D2;+0:9]-1>>[NH2;D1;+0:1]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[N;H0;D3;+0:9]1-[C:8]-[C:7]-[#16:6]-[C:5]-1-[c:4]
82.2
[{"value": 82.2, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(=O)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.2, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(=O)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A solution of 1.07 g of sodium isocyanate in 20 ml of water is added to a solution of 3.03 g of 2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine in 40 ml of ethanol, and 2.46 g of acetic acid are added thereto. The mixture is stirred at room temperature for 2 hours. 200 ml of water are added to the mixture,...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Urea
C1CSCN1
C1CSC[NH]1
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
null
O.C(C)O
null
2
[N-]=C=O.c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1>O.C(C)O>NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-eaa3856354d9479ba50679c11149fbdb
CCOC(=O)N=C=O.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1>>CCOC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
O.C(C)OC(=O)N=C=O.FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1.C([O-])([O-])=O.[K+].[K+].C(C)OC(=O)N=C=O>>C(C)OC(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F
[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]=[C:7]=[O:8].[NH:9]1[CH2:10][CH2:11][S:12][CH:13]1[c:14]1[cH:15][cH:16][cH:17][cH:18][c:19]1[O:20][CH2:21][CH2:22][N:23]1[CH2:24][CH2:25][N:26]([c:27]2[cH:28][cH:29][cH:30][c:31]([F:32])[cH:33]2)[CH2:34][CH2:35]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH:6][C:7](=[O:8])[N:9]1[CH2:10][CH2...
CCOC(=O)N=C=O.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1
CCOC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
O1CCCC1
Protection
Urea synthesis via isocyanate and secondary amine
af73464e4ca701ed477f99651384f5203ed9f16c6f2ea7c05a137da8d8037a87
1577e03da21f550f17923074b07cedede3bd99110f882d7bcf67bf5b974e59bc
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7].[c:8]-[C:9]1-[#16:10]-[C:11]-[C:12]-[NH;D2;+0:13]-1>>[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[N;H0;D3;+0:13]1-[C:12]-[C:11]-[#16:10]-[C:9]-1-[c:8]
40.5
[{"value": 40.5, "product": "C(C)OC(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
0.9 g of ethoxycarbonyl isocyanate is added to a solution of 2 g of 2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine in 30 ml of tetrahydrofuran, and the mixture is stirred at room temperature for 18 hours. 3.1 g of ethoxycarbonyl isocyanate are added to the mixture, and the mixture is stirred at ...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Secondary amine
Carbamic ester.Urea
C1CSCN1
C1CSC[NH]1
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
null
O1CCCC1
null
18
CCOC(=O)N=C=O.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1>O1CCCC1>CCOC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-4309e47a359d4d8aa7980c2c2a42a140
CS(=O)(=O)N=C=O.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1>>CS(=O)(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1.CS(=O)(=O)N=C=O>>CS(=O)(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F
[CH3:1][S:2](=[O:3])(=[O:4])[N:5]=[C:6]=[O:7].[NH:8]1[CH2:9][CH2:10][S:11][CH:12]1[c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[O:19][CH2:20][CH2:21][N:22]1[CH2:23][CH2:24][N:25]([c:26]2[cH:27][cH:28][cH:29][c:30]([F:31])[cH:32]2)[CH2:33][CH2:34]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][S:11]...
CS(=O)(=O)N=C=O.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1
CS(=O)(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
CC(=O)C
Acylation
Urea synthesis via isocyanate and secondary amine
4fc60b9212e2cd5fef4065a865923d912e694348c230069e34894dd7a40b5956
c54c1ed6f5693fe7284d99bae8ce6ef1af2bc669c2b604d5d1041c83f556df82
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
[C;D1;H3:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7].[c:8]-[C:9]1-[#16:10]-[C:11]-[C:12]-[NH;D2;+0:13]-1>>[C;D1;H3:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[N;H0;D3;+0:13]1-[C:12]-[C:11]-[#16:10]-[C:9]-1-[c:8]
61.3
[{"value": 61.3, "product": "CS(=O)(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
1.94 g of 2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine are dissolved in anhydrous acetone, and 0.73 g of methanesulfonyl isocyanate is added thereto at room temperature. After the mixture is stirred for 30 minutes, the mixture is concentrated under reduced pressure to remove solvent. The resid...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Sulfonamide.Urea
C1CSCN1
C1CSC[NH]1
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
null
CC(=O)C
null
0.5
CS(=O)(=O)N=C=O.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1>CC(=O)C>CS(=O)(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-1bfbce77124b4ef7b75e6c9cc7cb718a
CCP(=O)(CC)N=C=S.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1>>CCP(=O)(CC)NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
C(C)P(=O)(CC)N=C=S.FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1>>C(C)P(=O)(CC)NC(=S)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F
[CH3:1][CH2:2][P:3](=[O:4])([CH2:5][CH3:6])[N:7]=[C:8]=[S:9].[NH:10]1[CH2:11][CH2:12][S:13][CH:14]1[c:15]1[cH:16][cH:17][cH:18][cH:19][c:20]1[O:21][CH2:22][CH2:23][N:24]1[CH2:25][CH2:26][N:27]([c:28]2[cH:29][cH:30][cH:31][c:32]([F:33])[cH:34]2)[CH2:35][CH2:36]1>>[CH3:1][CH2:2][P:3](=[O:4])([CH2:5][CH3:6])[NH:7][C:8](=[...
CCP(=O)(CC)N=C=S.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1
CCP(=O)(CC)NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
CC(=O)C
Heteroatom Alkylation and Arylation
OtherReaction
db6efd8caa332621bc2f47da956ab9d93842b9ec246a2813d78b4744edee689e
48e0e6261e922bdea79c78ea511461d733cbd49c10100c782d86c83675c4be7c
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
[C:1]-[#15:2](-[C:3])(=[O;D1;H0:4])-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[S;D1;H0:7].[c:8]-[C:9]1-[#16:10]-[C:11]-[C:12]-[NH;D2;+0:13]-1>>[C:1]-[#15:2](-[C:3])(=[O;D1;H0:4])-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[S;D1;H0:7])-[N;H0;D3;+0:13]1-[C:12]-[C:11]-[#16:10]-[C:9]-1-[c:8]
85.2
[{"value": 81.0, "product": "C(C)P(=O)(CC)NC(=S)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 85.2, "product": "C(C)P(=O)(CC)NC(=S)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
DAY
0.68 g of diethylphosphoryl isothiocyanate is added to a solution of 1.23 g of 2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine in 20 ml of acetone, and the mixture is stirred for one day. The mixture is concentrated under reduced pressure to remove solvent. The residue is extracted with chlorofor...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Isothiocyanate
Thiourea
C1CSCN1
C1CSC[NH]1
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
null
CC(=O)C
null
24
CCP(=O)(CC)N=C=S.Fc1cccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)c1>CC(=O)C>CCP(=O)(CC)NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-cc5689b69bf7423889aa61414394c6d6
CC(=O)Cl.CNC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>>CC(=O)N(C)C(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
C(C)(=O)Cl.[H-].[Na+].CNC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F>>C(C)(=O)N(C(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F)C
Cl[C:2]([CH3:1])=[O:3].[NH:4]([CH3:5])[C:6](=[O:7])[N:8]1[CH2:9][CH2:10][S:11][CH:12]1[c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[O:19][CH2:20][CH2:21][N:22]1[CH2:23][CH2:24][N:25]([c:26]2[cH:27][cH:28][cH:29][c:30]([F:31])[cH:32]2)[CH2:33][CH2:34]1>>[CH3:1][C:2](=[O:3])[N:4]([CH3:5])[C:6](=[O:7])[N:8]1[CH2:9][CH2:10][S...
CC(=O)Cl.CNC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
CC(=O)N(C)C(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
CCOCC.CN(C=O)C
Acylation
N-alkylation of secondary amines with alkyl halides
996e0ddf2d6b57ad6b8e08b45c57ed86da0355f61815643564e670f244fe345b
ed2e2a2113014ef864b0a3bd063f004647b373e1f6820e0fdd5587d12a0e8460
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
Cl-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[#16:4]-[C:5]-[#7:6](-[C:7](=[O;D1;H0:8])-[NH;D2;+0:9]-[C;D1;H3:10])-[C:11]>>[#16:4]-[C:5]-[#7:6](-[C:7](=[O;D1;H0:8])-[N;H0;D3;+0:9](-[C;D1;H3:10])-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3])-[C:11]
null
[]
50
CELSIUS
20
HOUR
0.1 g of sodium hydride (60% oil dispersion) is added to a solution of one g of N-methyl-2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboxamide in 30 ml of dimethylformamide, and a solution of 0.19 g of acetyl chloride in 5 ml of ether is added thereto. After the mixture is stirred at 50° ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Urea
Urea.Substituted dicarboximide
null
null
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HCl
CCOCC.CN(C=O)C
50
20
CC(=O)Cl.CNC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>CCOCC.CN(C=O)C>CC(=O)N(C)C(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-32f84dbb0b9d4ce7a27403d9bb0ba450
CCC(=O)Cl.CNC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>>CCC(=O)N(C)C(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
CNC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F.C(CC)(=O)Cl.C(C)N(CC)CC>>CN(C(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F)C(CC)=O
Cl[C:3]([CH2:2][CH3:1])=[O:4].[NH:5]([CH3:6])[C:7](=[O:8])[N:9]1[CH2:10][CH2:11][S:12][CH:13]1[c:14]1[cH:15][cH:16][cH:17][cH:18][c:19]1[O:20][CH2:21][CH2:22][N:23]1[CH2:24][CH2:25][N:26]([c:27]2[cH:28][cH:29][cH:30][c:31]([F:32])[cH:33]2)[CH2:34][CH2:35]1>>[CH3:1][CH2:2][C:3](=[O:4])[N:5]([CH3:6])[C:7](=[O:8])[N:9]1[C...
CCC(=O)Cl.CNC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
CCC(=O)N(C)C(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
C1(=CC=CC=C1)C
Acylation
N-alkylation of secondary amines with alkyl halides
996e0ddf2d6b57ad6b8e08b45c57ed86da0355f61815643564e670f244fe345b
ed2e2a2113014ef864b0a3bd063f004647b373e1f6820e0fdd5587d12a0e8460
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C;D1;H3:4].[#16:5]-[C:6]-[#7:7](-[C:8](=[O;D1;H0:9])-[NH;D2;+0:10]-[C;D1;H3:11])-[C:12]>>[#16:5]-[C:6]-[#7:7](-[C:8](=[O;D1;H0:9])-[N;H0;D3;+0:10](-[C;D1;H3:11])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C;D1;H3:4])-[C:12]
12
[{"value": 12.0, "product": "CN(C(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F)C(CC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 2.22 g of N-methyl-2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboxamide, 1.39 g of propionyl chloride, 2.53 g of triethylamine and 50 ml of toluene is refluxed for 2.5 days with stirring. The mixture is concentrated under reduced pressure to remove solvent. Water is added to...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Urea
Urea.Substituted dicarboximide
null
null
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HCl
C1(=CC=CC=C1)C
null
null
CCC(=O)Cl.CNC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>C1(=CC=CC=C1)C>CCC(=O)N(C)C(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-7c55a82908a04847bac89c1a561b1980
CC(=O)Cl.CC(=O)Cl.NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>>CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(=O)N.O1CCCC1.C(C)N(CC)CC.C(C)(=O)Cl.C(C)N(CC)CC.C(C)(=O)Cl.O1CCCC1>>C(C)(=O)N=C(OC(C)=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F
Cl[C:2]([CH3:1])=[O:3].Cl[C:7]([CH3:8])=[O:9].[NH2:4][C:5](=[O:6])[N:10]1[CH2:11][CH2:12][S:13][CH:14]1[c:15]1[cH:16][cH:17][cH:18][cH:19][c:20]1[O:21][CH2:22][CH2:23][N:24]1[CH2:25][CH2:26][N:27]([c:28]2[cH:29][cH:30][cH:31][c:32]([F:33])[cH:34]2)[CH2:35][CH2:36]1>>[CH3:1][C:2](=[O:3])[N:4]=[C:5]([O:6][C:7]([CH3:8])=[...
CC(=O)Cl.CC(=O)Cl.NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
null
Acylation
OtherReaction
7cbab782ac1731d55afce8259d9230a293eafaaf2c8590fb5b21395b8697a775
24b7119c60fa8babfa147854c12206b2a2e456f249b6d16380d6c202d29d17da
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
Cl-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].Cl-[C;H0;D3;+0:4](-[C;D1;H3:5])=[O;D1;H0:6].[#16:7]-[C:8]-[#7:9](-[C;H0;D3;+0:10](-[NH2;D1;+0:11])=[O;H0;D1;+0:12])-[C:13]>>[#16:7]-[C:8]-[#7:9](-[C;H0;D3;+0:10](=[N;H0;D2;+0:11]-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3])-[O;H0;D2;+0:12]-[C;H0;D3;+0:4](-[C;D1;H3:5])=[O;D1;H0:6...
56
[{"value": 56.0, "product": "C(C)(=O)N=C(OC(C)=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3
DAY
1.08 g of 2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboxamide are dissolved in 20 ml of tetrahydrofuran, and 0.76 g of triethylamine is added thereto. A solution of 0.59 g of acetyl chloride in one ml of tetrahydrofuran is added to the mixture under ice-cooling, and the mixture is stirr...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Urea
Ester
null
null
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HCl
null
null
72
CC(=O)Cl.CC(=O)Cl.NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>>CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-d0bb55d299664209bdb4fb168a9ad2a8
CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>>CC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
C(C)(=O)N=C(OC(C)=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F.Cl>>C(C)(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F
CC(=O)[O:6][C:5](=[N:4][C:2]([CH3:1])=[O:3])[N:7]1[CH2:8][CH2:9][S:10][CH:11]1[c:12]1[cH:13][cH:14][cH:15][cH:16][c:17]1[O:18][CH2:19][CH2:20][N:21]1[CH2:22][CH2:23][N:24]([c:25]2[cH:26][cH:27][cH:28][c:29]([F:30])[cH:31]2)[CH2:32][CH2:33]1>>[CH3:1][C:2](=[O:3])[NH:4][C:5](=[O:6])[N:7]1[CH2:8][CH2:9][S:10][CH:11]1[c:12...
CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
CC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
O1CCCC1.[OH-].[Na+].C(C)O
Miscellaneous
OtherReaction
2e6fb0a3329693eca9c08ec9ab0da418063be847a6c403d46e63c08fc5041693
82a707dbab5460decf10b063efbab9ed39707af4af5e33ed675afdf1c19138af
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
C-C(=O)-[O;H0;D2;+0:1]-[C;H0;D3;+0:2](=[N;H0;D2;+0:3]-[C:4](-[C;D1;H3:5])=[O;D1;H0:6])-[#7:7](-[C:8])-[C:9]-[#16:10]>>[#16:10]-[C:9]-[#7:7](-[C;H0;D3;+0:2](=[O;H0;D1;+0:1])-[NH;D2;+0:3]-[C:4](-[C;D1;H3:5])=[O;D1;H0:6])-[C:8]
90.4
[{"value": 90.0, "product": "C(C)(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.4, "product": "C(C)(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
0.59 g of N,O-diacetyl-2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboximidic acid is dissolved in a mixture of 15 ml of ethanol and 5 ml of tetrahydrofuran, and 1.34 ml of 10% aqueous sodium hydroxide solution is added thereto under ice-cooling. The mixture is stirred for 15 minutes, and...
10.6084/m9.figshare.5104873.v1
null
Ester
Urea
null
null
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HO-
O1CCCC1.[OH-].[Na+].C(C)O
null
0.25
CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>O1CCCC1.[OH-].[Na+].C(C)O>CC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-aa76061cb7944db687e41e7774788579
CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1>>CC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
Cl.C(C)(=O)N=C(OC(C)=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC=CC=C1.C(C)O.[OH-].[Na+]>>C(C)(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC=CC=C1
CC(=O)[O:6][C:5](=[N:4][C:2]([CH3:1])=[O:3])[N:7]1[CH2:8][CH2:9][S:10][CH:11]1[c:12]1[cH:13][cH:14][cH:15][cH:16][c:17]1[O:18][CH2:19][CH2:20][N:21]1[CH2:22][CH2:23][N:24]([c:25]2[cH:26][cH:27][cH:28][cH:29][cH:30]2)[CH2:31][CH2:32]1>>[CH3:1][C:2](=[O:3])[NH:4][C:5](=[O:6])[N:7]1[CH2:8][CH2:9][S:10][CH:11]1[c:12]1[cH:1...
CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
CC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
null
null
O1CCCC1.O
Miscellaneous
OtherReaction
2e6fb0a3329693eca9c08ec9ab0da418063be847a6c403d46e63c08fc5041693
82a707dbab5460decf10b063efbab9ed39707af4af5e33ed675afdf1c19138af
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
C-C(=O)-[O;H0;D2;+0:1]-[C;H0;D3;+0:2](=[N;H0;D2;+0:3]-[C:4](-[C;D1;H3:5])=[O;D1;H0:6])-[#7:7](-[C:8])-[C:9]-[#16:10]>>[#16:10]-[C:9]-[#7:7](-[C;H0;D3;+0:2](=[O;H0;D1;+0:1])-[NH;D2;+0:3]-[C:4](-[C;D1;H3:5])=[O;D1;H0:6])-[C:8]
66.1
[{"value": 66.1, "product": "C(C)(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 66.1, "product": "C(C)(=O)NC(=O)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
A mixture of 1.19 g of N,O-diacetyl-2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboximidic acid, 20 ml of ethanol, 0.287 g of sodium hydroxide, 2.7 ml of water and 20 ml of tetrahydrofuran is stirred for 1.5 hours under ice-cooling. The mixture is neutralized with 10% hydrochloric acid, and the mix...
10.6084/m9.figshare.5104873.v1
null
Ester
Urea
null
null
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HO-
O1CCCC1.O
null
1.5
CC(=O)N=C(OC(C)=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1>O1CCCC1.O>CC(=O)NC(=O)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-f2ba0d33acd149c78f546b6cef92101a
CC(=O)NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>>NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
C(C)(=O)NC(=S)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC(=CC=C1)F.[OH-].[Na+]>>FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(N)=S
CC(=O)[NH:1][C:2](=[S:3])[N:4]1[CH2:5][CH2:6][S:7][CH:8]1[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[O:15][CH2:16][CH2:17][N:18]1[CH2:19][CH2:20][N:21]([c:22]2[cH:23][cH:24][cH:25][c:26]([F:27])[cH:28]2)[CH2:29][CH2:30]1>>[NH2:1][C:2](=[S:3])[N:4]1[CH2:5][CH2:6][S:7][CH:8]1[c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[O:15][...
CC(=O)NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
null
null
C(C)O
Reduction
Hydrogenolysis of amides/imides/carbamates
b7ab3e4f878ec88ccf9f24aa8ace9c0e9bd79c45879c7956fca4b89bfcf032d3
eb308e50ea59a818e9be36da7e60c01d0f7ab2d0f39e89f35847ab33b6eb422f
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
C-C(=O)-[NH;D2;+0:1]-[C:2](=[S;D1;H0:3])-[#7:4](-[C:5])-[C:6]-[#16:7]>>[#16:7]-[C:6]-[#7:4](-[C:2](-[NH2;D1;+0:1])=[S;D1;H0:3])-[C:5]
90
[{"value": 90.0, "product": "FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(N)=S", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.0, "product": "FC=1C=C(C=CC1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1C(N)=S", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 2.87 g of N-acetyl-2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carbothioamide, 7.3 ml of 10% aqueous sodium hydroxide solution and 60 ml of ethanol is refluxed for 20 hours and then concentrated under reduced pressure to remove solvent. The residue is extracted with ethyl aceta...
10.6084/m9.figshare.5104873.v1
null
Thiourea.Secondary amide
Thiourea
null
null
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HO-
C(C)O
null
null
CC(=O)NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1>C(C)O>NC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2cccc(F)c2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-63d52bf819e7416a9fcd3ec481ab9c00
CN(C(=O)C1CCCN1S(=O)(=O)c1ccc2ccccc2c1)C(=S)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1>>CNC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
CN(C(=S)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC=CC=C1)C(=O)C1N(CCC1)S(=O)(=O)C1=CC2=CC=CC=C2C=C1.O1CCCC1.CO.[OH-].[Na+]>>CNC(=S)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC=CC=C1
O=C(C1CCCN1S(=O)(=O)c1ccc2ccccc2c1)[N:2]([CH3:1])[C:3](=[S:4])[N:5]1[CH2:6][CH2:7][S:8][CH:9]1[c:10]1[cH:11][cH:12][cH:13][cH:14][c:15]1[O:16][CH2:17][CH2:18][N:19]1[CH2:20][CH2:21][N:22]([c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[CH2:29][CH2:30]1>>[CH3:1][NH:2][C:3](=[S:4])[N:5]1[CH2:6][CH2:7][S:8][CH:9]1[c:10]1[cH:...
CN(C(=O)C1CCCN1S(=O)(=O)c1ccc2ccccc2c1)C(=S)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
CNC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
null
null
O
Reduction
Hydrogenolysis of tertiary amines
4c88e43287aa5278815bca89984947d8fc6205bb3075a9603648c7c1700411ed
5d07a16126cebdc2b1f430d06d117de6ba73811a47aaf39b506886f5cb1149fd
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
O=C(-C1-C-C-C-N-1-S(=O)(=O)-c1:c:c:c2:c:c:c:c:c:2:c:1)-[N;H0;D3;+0:1](-[C;D1;H3:2])-[C:3](=[S;D1;H0:4])-[#7:5](-[C:6])-[C:7]-[#16:8]>>[#16:8]-[C:7]-[#7:5](-[C:3](=[S;D1;H0:4])-[NH;D2;+0:1]-[C;D1;H3:2])-[C:6]
94.2
[{"value": 94.2, "product": "CNC(=S)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 94.2, "product": "CNC(=S)N1C(SCC1)C1=C(C=CC=C1)OCCN1CCN(CC1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
1.05 g of (-)-N-methyl-N-[1-(2-naphthylsulfonyl)pyrrolidine-2-carbonyl]-2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carbothioamide, 40 ml of tetrahydrofuran, 40 ml of methanol, 120 mg of sodium hydroxide and 3 ml of water are treated in the same manner as described in Example 148-(2). 600 mg of (-)-N...
10.6084/m9.figshare.5104873.v1
null
Thiourea.Tertiary amide.Tertiary amine
Thiourea
C1CCNC1.c1ccc2ccccc2c1
null
C1CSC[NH]1.c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HO-
O
null
null
CN(C(=O)C1CCCN1S(=O)(=O)c1ccc2ccccc2c1)C(=S)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1>O>CNC(=S)N1CCSC1c1ccccc1OCCN1CCN(c2ccccc2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-0a61adb5089146bbaafb86e29a4c179b
Cc1ccc(S(=O)(=O)OCCCl)cc1.O=Cc1ccccc1O>>O=Cc1ccccc1OCCCl
OC1=C(C=O)C=CC=C1.ClCCOS(=O)(=O)C1=CC=C(C)C=C1.C([O-])([O-])=O.[K+].[K+]>>ClCCOC1=C(C=O)C=CC=C1
Cc1ccc(S(=O)(=O)O[CH2:10][CH2:11][Cl:12])cc1.[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[OH:9]>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[O:9][CH2:10][CH2:11][Cl:12]
Cc1ccc(S(=O)(=O)OCCCl)cc1.O=Cc1ccccc1O
O=Cc1ccccc1OCCCl
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
b5213736859cf91483a02f350869986d9b7674724716adef8a5d7a4bbdb79574
3d107e624e135e10014c7bf413dd0be27e1e4488f039e545b94cb1680b764158
c1ccccc1
C-c1:c:c:c(-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[Cl;D1;H0:3]):c:c:1.[O;D1;H0:4]=[C:5]-[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]>>[Cl;D1;H0:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:8]-[c:7](:[c:9]):[c:6]-[C:5]=[O;D1;H0:4]
86
[{"value": 86.0, "product": "ClCCOC1=C(C=O)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 85.8, "product": "ClCCOC1=C(C=O)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
DAY
40.0 g of 2-hydroxybenzaldehyde, 84 g of 1-chloro-2-tosyloxyethane and 50 g of potassium carbonate are added to 270 ml of dimethylformamide, and the mixture is stirred at room temperature for 3 days. After the reaction, half of the solvent is removed under reduced pressure. About 600 ml of water are added to the residu...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Aromatic alcohol
Ether
c1ccccc1
null
c1ccccc1
TsOH.HO-
CN(C=O)C
null
72
Cc1ccc(S(=O)(=O)OCCCl)cc1.O=Cc1ccccc1O>CN(C=O)C>O=Cc1ccccc1OCCCl
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-a487da4d0ad342668dd109913a8681fe
CNC(=S)N1CCSC1c1ccc(O)cc1.Cc1ccc(S(=O)(=O)OCCCl)cc1>>CNC(=S)N1CCSC1c1ccc(OCCCl)cc1
CNC(=S)N1C(SCC1)C1=CC=C(C=C1)O.ClCCOS(=O)(=O)C1=CC=C(C)C=C1.C([O-])([O-])=O.[K+].[K+]>>CNC(=S)N1C(SCC1)C1=CC=C(C=C1)OCCCl
[CH3:1][NH:2][C:3](=[S:4])[N:5]1[CH2:6][CH2:7][S:8][CH:9]1[c:10]1[cH:11][cH:12][c:13]([OH:14])[cH:18][cH:19]1.Cc1ccc(S(=O)(=O)O[CH2:15][CH2:16][Cl:17])cc1>>[CH3:1][NH:2][C:3](=[S:4])[N:5]1[CH2:6][CH2:7][S:8][CH:9]1[c:10]1[cH:11][cH:12][c:13]([O:14][CH2:15][CH2:16][Cl:17])[cH:18][cH:19]1
CNC(=S)N1CCSC1c1ccc(O)cc1.Cc1ccc(S(=O)(=O)OCCCl)cc1
CNC(=S)N1CCSC1c1ccc(OCCCl)cc1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
b5213736859cf91483a02f350869986d9b7674724716adef8a5d7a4bbdb79574
3d107e624e135e10014c7bf413dd0be27e1e4488f039e545b94cb1680b764158
c1ccc(C2NCCS2)cc1
C-c1:c:c:c(-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[Cl;D1;H0:3]):c:c:1.[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[Cl;D1;H0:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
51.9
[{"value": 51.9, "product": "CNC(=S)N1C(SCC1)C1=CC=C(C=C1)OCCCl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 49.4, "product": "CNC(=S)N1C(SCC1)C1=CC=C(C=C1)OCCCl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
DAY
A mixture of 5 g of N-methyl-2-(4-hydroxyphenyl)thiazolidine-3-carbothioamide, 4.6 g of 1-chloro-2-tosyloxyethane, 4 g of potassium carbonate and 20 ml of dimethylformamide is stirred at room temperature for 2 days and further stirred at 50° C. for 20 hours. The mixture is concentrated under reduced pressure to remove ...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Aromatic alcohol
Ether
c1ccccc1
null
C1CSC[NH]1.c1ccccc1
TsOH.HO-
CN(C=O)C
null
48
CNC(=S)N1CCSC1c1ccc(O)cc1.Cc1ccc(S(=O)(=O)OCCCl)cc1>CN(C=O)C>CNC(=S)N1CCSC1c1ccc(OCCCl)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-1ab0649934ff468ca3ce4dfc173e5293
ClCCCBr.OCc1ccccc1S>>OCc1ccccc1SCCCCl
OCC1=C(C=CC=C1)S.BrCCCCl.C([O-])([O-])=O.[K+].[K+]>>ClCCCSC1=C(CO)C=CC=C1
Br[CH2:10][CH2:11][CH2:12][Cl:13].[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[SH:9]>>[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[S:9][CH2:10][CH2:11][CH2:12][Cl:13]
ClCCCBr.OCc1ccccc1S
OCc1ccccc1SCCCCl
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
thioether_nucl_sub
26df88c6a3f5f203c89584658be4e126cb42994c98a2e16bc812e1036cdae857
8b2f52296c3a93039174c980b6042ba15754e04d6892a1284c3a32985220b214
c1ccccc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[SH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
93
[{"value": 93.0, "product": "ClCCCSC1=C(CO)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.3, "product": "ClCCCSC1=C(CO)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A mixture of 11.9 g of 2-(hydroxymethyl)thiophenol, 35.44 g of 1-bromo-3-chloropropane, 11.58 g of potassium carbonate and 150 ml of dimethylformamide is stirred at room temperature for 2 hours. Insoluble materials are filtered off, and the filtrate is concentrated under reduced pressure to remove solvent. Water is add...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic thiol
Monosulfide
null
null
c1ccccc1
HBr
CN(C=O)C
null
2
ClCCCBr.OCc1ccccc1S>CN(C=O)C>OCc1ccccc1SCCCCl
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-60e4dc598c6f440faebfb4ac0e619073
COC(=O)c1ccc(SCCCCl)cc1>>OCc1ccc(SCCCCl)cc1
[H-].[Al+3].[Li+].[H-].[H-].[H-].ClCCCSC1=CC=C(C(=O)OC)C=C1.O>>ClCCCSC1=CC=C(CO)C=C1
CO[C:2](=[O:1])[c:3]1[cH:4][cH:5][c:6]([S:7][CH2:8][CH2:9][CH2:10][Cl:11])[cH:12][cH:13]1>>[OH:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([S:7][CH2:8][CH2:9][CH2:10][Cl:11])[cH:12][cH:13]1
COC(=O)c1ccc(SCCCCl)cc1
OCc1ccc(SCCCCl)cc1
null
null
O1CCCC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccccc1
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3](:[c:4]):[c:5]>>[OH;D1;+0:2]-[CH2;D2;+0:1]-[c:3](:[c:4]):[c:5]
85.3
[{"value": 85.3, "product": "ClCCCSC1=CC=C(CO)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
45
MINUTE
5 g of lithium aluminum hydride are suspended in 200 ml of tetrahydrofuran, and a solution of 31.9 g of methyl 4-(3-chloro-propylthio)benzoate in 200 ml of tetrahydrofuran is added thereto at 5° to 15° C. The mixture is stirred at the same temperature for 45 minutes. Water is added to the mixture at a temperature of be...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccccc1
Other
O1CCCC1
null
0.75
COC(=O)c1ccc(SCCCCl)cc1>O1CCCC1>OCc1ccc(SCCCCl)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-7f4ccdacd2124c509852605e00d848bd
OCc1ccccc1SCCCl>>O=Cc1ccccc1SCCCl
CS(=O)C.C(C(=O)Cl)(=O)Cl.C(C)N(CC)CC.ClCCSC1=C(CO)C=CC=C1>>ClCCSC1=C(C=O)C=CC=C1
[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[S:9][CH2:10][CH2:11][Cl:12]>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[S:9][CH2:10][CH2:11][Cl:12]
OCc1ccccc1SCCCl
O=Cc1ccccc1SCCCl
null
null
O.C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccccc1
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]
91.7
[{"value": 91.6, "product": "ClCCSC1=C(C=O)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.7, "product": "ClCCSC1=C(C=O)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
A solution of 27.8 g of dimethylsulfoxide in 50 ml of methylene chloride is added to a solution of 22.6 g of oxalyl chloride in 450 ml of methylene chloride at -60° C. during one hour, and a solution of 32.7 g of 2-(2-chloroethylthio)benzylalcohol in 50 ml of methylene chloride is added thereto. The mixture is stirred ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccccc1
null
O.C(Cl)Cl
null
0.25
OCc1ccccc1SCCCl>O.C(Cl)Cl>O=Cc1ccccc1SCCCl
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-84c56ccc3d8f4af7b42a8396c4f681d0
ClCCCN1CCN(c2ccccc2)CC1.O=Cc1ccccc1O>>O=Cc1ccccc1OCCCN1CCN(c2ccccc2)CC1
[Na].OC1=C(C=O)C=CC=C1.Cl.Cl.ClCCCN1CCN(CC1)C1=CC=CC=C1.C([O-])([O-])=O.[K+].[K+]>>C1(=CC=CC=C1)N1CCN(CC1)CCCOC1=C(C=O)C=CC=C1
Cl[CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][N:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[CH2:23][CH2:24]1.[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[OH:9]>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[O:9][CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][N:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:...
ClCCCN1CCN(c2ccccc2)CC1.O=Cc1ccccc1O
O=Cc1ccccc1OCCCN1CCN(c2ccccc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccc(OCCCN2CCN(c3ccccc3)CC2)cc1
Cl-[CH2;D2;+0:1]-[C:2]-[C:3].[O;D1;H0:4]=[C:5]-[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:8]-[c:7](:[c:9]):[c:6]-[C:5]=[O;D1;H0:4]
74.4
[{"value": 74.4, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCCOC1=C(C=O)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
HOUR
A mixture of 3.88 g of 2-hydroxybenzaldehyde sodium salt, 7.00 g of 1-(3-chloropropyl)-4-phenylpiperazine dihydrochloride, 6.80 g of potassium carbonate and 50 ml of dimethylformamide is stirred at 60° to 70° C. for 15 hours under nitrogen atmosphere, and is concentrated under reduced pressure to remove solvent. Water ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HCl
CN(C=O)C
null
15
ClCCCN1CCN(c2ccccc2)CC1.O=Cc1ccccc1O>CN(C=O)C>O=Cc1ccccc1OCCCN1CCN(c2ccccc2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-f5b0b9287b1249399995fc70dd4ff6e7
O=Cc1ccccc1OCCCl.OCCO>>ClCCOc1ccccc1C1OCCO1
C([O-])(O)=O.[Na+].ClCCOC1=C(C=O)C=CC=C1.C(CO)O.P(O)(O)(O)=O>>C1COC(C2=C(C=CC=C2)OCCCl)O1
[Cl:1][CH2:2][CH2:3][O:4][c:5]1[cH:6][cH:7][cH:8][cH:9][c:10]1[CH:11]=[O:12].O[CH2:13][CH2:14][OH:15]>>[Cl:1][CH2:2][CH2:3][O:4][c:5]1[cH:6][cH:7][cH:8][cH:9][c:10]1[CH:11]1[O:12][CH2:13][CH2:14][O:15]1
O=Cc1ccccc1OCCCl.OCCO
ClCCOc1ccccc1C1OCCO1
null
null
C1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
fe0fbb45a87f24c1e456c6b4e41101562cd8f0af3ec376bb6115e7c1555d997b
7ac65b5a5f576337ce8e86e0130eb9b4757ca21b2419a0e82bbdfd5def30ee73
c1ccc(C2OCCO2)cc1
O-[CH2;D2;+0:1]-[C:2]-[OH;D1;+0:3].[O;H0;D1;+0:4]=[CH;D2;+0:5]-[c:6](:[c:7]):[c:8]>>[c:7]:[c:6](-[CH;D3;+0:5]1-[O;H0;D2;+0:4]-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-1):[c:8]
97.2
[{"value": 97.0, "product": "C1COC(C2=C(C=CC=C2)OCCCl)O1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.2, "product": "C1COC(C2=C(C=CC=C2)OCCCl)O1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
To a solution of 46.5 g of 2-(2-chloroethyloxy)benzaldehyde and 33.2 g of ethylene glycol in 500 ml of benzene in added 0.5 ml of 85% phosphoric acid, and the mixture is refluxed with stirring for about 18 hours while removing the produced water. After the reaction, the reaction mixture is cooled with ice and is made a...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary alcohol.Primary alcohol
Ether.Ether
null
C1COCO1
c1ccccc1.C1COCO1
HO-
C1=CC=CC=C1
null
18
O=Cc1ccccc1OCCCl.OCCO>C1=CC=CC=C1>ClCCOc1ccccc1C1OCCO1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-5ac80b0aa0e5432ea6f8cf1cb67bf4af
ClCCOc1ccccc1C1OCCO1.c1ccc(N2CCNCC2)cc1>>O=Cc1ccccc1OCCN1CCN(c2ccccc2)CC1
C1COC(C2=C(C=CC=C2)OCCCl)O1.C1(=CC=CC=C1)N1CCNCC1.C([O-])([O-])=O.[K+].[K+]>>C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=O)C=CC=C1
Cl[CH2:11][CH2:10][O:9][c:8]1[c:3]([CH:2]2OCC[O:1]2)[cH:4][cH:5][cH:6][cH:7]1.[NH:12]1[CH2:13][CH2:14][N:15]([c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:22][CH2:23]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[O:9][CH2:10][CH2:11][N:12]1[CH2:13][CH2:14][N:15]([c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:...
ClCCOc1ccccc1C1OCCO1.c1ccc(N2CCNCC2)cc1
O=Cc1ccccc1OCCN1CCN(c2ccccc2)CC1
null
null
CN(C=O)C
Acylation
OtherReaction
e4ef4aeaaf8934513c8e22bceb9f0c076aecff470acc174043e72c9f596892d3
3fea7cb017cc7c3c2d30466649a837ff1527347fa4d748b5fc13e5f58792738d
c1ccc(OCCN2CCN(c3ccccc3)CC2)cc1
Cl-[CH2;D2;+0:1]-[C:2]-[#8:3]-[c:4]:[c:5](-[CH;D3;+0:6]1-O-C-C-[O;H0;D2;+0:7]-1):[c:8].[#7:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[O;H0;D1;+0:7]=[CH;D2;+0:6]-[c:5](:[c:8]):[c:4]-[#8:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:12]1-[C:11]-[C:10]-[#7:9]-[C:14]-[C:13]-1
42.8
[{"value": 42.8, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=O)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A suspension of 2.29 g of 2-(2-chloroethyloxy)benzaldehyde ethyleneacetal, 1.73 g of N-phenylpiperazine, 1.50 g of anhyrous potassium carbonate and 15 ml of dimethylformamide is stirred at 70°-80° C. for about 18 hours under argon atmosphere. The reaction mixture is concentrated under reduced pressure to remove dimethy...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Secondary amine
Aldehyde.Tertiary amine
C1COCO1.C1CNCC[NH]1
C1C[NH]CC[NH]1
c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HCl
CN(C=O)C
null
18
ClCCOc1ccccc1C1OCCO1.c1ccc(N2CCNCC2)cc1>CN(C=O)C>O=Cc1ccccc1OCCN1CCN(c2ccccc2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-55e7ad6b22ff44e29d699b8a2b766ad4
ClCCCN1CCN(c2ccccc2)CC1.OCc1ccccc1S>>OCc1ccccc1SCCCN1CCN(c2ccccc2)CC1
OCC1=C(C=CC=C1)S.Cl.Cl.ClCCCN1CCN(CC1)C1=CC=CC=C1.C([O-])([O-])=O.[K+].[K+]>>C1(=CC=CC=C1)N1CCN(CC1)CCCSC1=C(CO)C=CC=C1
Cl[CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][N:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[CH2:23][CH2:24]1.[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[SH:9]>>[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[S:9][CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][N:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][c...
ClCCCN1CCN(c2ccccc2)CC1.OCc1ccccc1S
OCc1ccccc1SCCCN1CCN(c2ccccc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
thioether_nucl_sub
26df88c6a3f5f203c89584658be4e126cb42994c98a2e16bc812e1036cdae857
8b2f52296c3a93039174c980b6042ba15754e04d6892a1284c3a32985220b214
c1ccc(SCCCN2CCN(c3ccccc3)CC2)cc1
Cl-[CH2;D2;+0:1]-[C:2]-[C:3].[SH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
91
[{"value": 91.0, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCCSC1=C(CO)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.7, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCCSC1=C(CO)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
6
HOUR
A mixture of 1.56 g of 2-(hydroxymethyl)thiophenol, 3.77 g of 1-(3-chloropropyl)-4-phenylpiperazine dihydrochloride, 5.02 g of potassium carbonate and 40 ml of dimethylformamide is stirred at 50° C. for 6 hours. Insoluble materials are filtered off, and the filtrate is concentrated under reduced pressure to remove solv...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic thiol
Monosulfide
null
null
c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
HCl
CN(C=O)C
50
6
ClCCCN1CCN(c2ccccc2)CC1.OCc1ccccc1S>CN(C=O)C>OCc1ccccc1SCCCN1CCN(c2ccccc2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-e1eec7f7add74932a65c6586620a67b0
OCc1ccccc1SCCCN1CCN(c2ccccc2)CC1>>O=Cc1ccccc1SCCCN1CCN(c2ccccc2)CC1
C(C)N(CC)CC.CS(=O)C.C(C(=O)Cl)(=O)Cl.C1(=CC=CC=C1)N1CCN(CC1)CCCSC1=C(CO)C=CC=C1>>C1(=CC=CC=C1)N1CCN(CC1)CCCSC1=C(C=O)C=CC=C1
[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[S:9][CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][N:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[CH2:23][CH2:24]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[S:9][CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][N:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]...
OCc1ccccc1SCCCN1CCN(c2ccccc2)CC1
O=Cc1ccccc1SCCCN1CCN(c2ccccc2)CC1
null
null
O.C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccc(SCCCN2CCN(c3ccccc3)CC2)cc1
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]
90.5
[{"value": 90.5, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCCSC1=C(C=O)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.5, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCCSC1=C(C=O)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
A solution of 1.1 g of dimethylsulfoxide in 5 ml of methylene chloride is added to a solution of 0.894 g of oxalyl chloride in 20 ml of methylene chloride at -50° C. A solution of 2.19 g of 2-[3-(4-phenylpiperazin-1-yl)propylthio]benzylalcohol in 10 ml of methylene chloride is added to the mixture at -50° C., and the m...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
null
O.C(Cl)Cl
null
0.25
OCc1ccccc1SCCCN1CCN(c2ccccc2)CC1>O.C(Cl)Cl>O=Cc1ccccc1SCCCN1CCN(c2ccccc2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-eb12f920bec740a89ef3f6602f83b842
OCc1ccccc1SCCN1CCN(c2ccccc2)CC1>>O=Cc1ccccc1SCCN1CCN(c2ccccc2)CC1
C1(=CC=CC=C1)N1CCN(CC1)CCSC1=C(CO)C=CC=C1.C(C(=O)Cl)(=O)Cl.CS(=O)C>>C1(=CC=CC=C1)N1CCN(CC1)CCSC1=C(C=O)C=CC=C1
[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[S:9][CH2:10][CH2:11][N:12]1[CH2:13][CH2:14][N:15]([c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:22][CH2:23]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[S:9][CH2:10][CH2:11][N:12]1[CH2:13][CH2:14][N:15]([c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:22][CH2:2...
OCc1ccccc1SCCN1CCN(c2ccccc2)CC1
O=Cc1ccccc1SCCN1CCN(c2ccccc2)CC1
null
null
C(C)N(CC)CC
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccc(SCCN2CCN(c3ccccc3)CC2)cc1
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]
93.1
[{"value": 93.0, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCSC1=C(C=O)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.1, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCSC1=C(C=O)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
6.0 g of 2-[2-(4-phenylpiperazin-1-yl)ethylthio]benzylalcohol, 2.60 g of oxalyl chloride, 3.2 g of dimethylsulfoxide and 9.3 g of triethylamine are treated in the same manner as described above. 5.55 g of 2-[2-(4-phenylpiperazin-1-yl)ethylthio]benzaldehyde are obtained. Yield: 93%. Conditions: See reaction.notes.proced...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
null
C(C)N(CC)CC
null
null
OCc1ccccc1SCCN1CCN(c2ccccc2)CC1>C(C)N(CC)CC>O=Cc1ccccc1SCCN1CCN(c2ccccc2)CC1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-46245ad98a7644dbbba7e7b2ed233ffd
NCCS.O=Cc1ccccc1OCCN1CCN(c2ccccc2)CC1>>c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=O)C=CC=C1.[OH-].[Na+].Cl.NCCS>>C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1
[NH2:19][CH2:20][CH2:21][SH:22].O=[CH:18][c:17]1[c:12]([O:11][CH2:10][CH2:9][N:8]2[CH2:7][CH2:6][N:5]([c:4]3[cH:3][cH:2][cH:1][cH:26][cH:25]3)[CH2:24][CH2:23]2)[cH:13][cH:14][cH:15][cH:16]1>>[cH:1]1[cH:2][cH:3][c:4]([N:5]2[CH2:6][CH2:7][N:8]([CH2:9][CH2:10][O:11][c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[CH:18]3[NH:19]...
NCCS.O=Cc1ccccc1OCCN1CCN(c2ccccc2)CC1
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
15efb05380d8debf7bab56597d1fa9b0622ee8622ff23260de9add0344b89365
5d87d269e927a5d4c4d7957f00c75ee007fdf5209a75b4d446e6fde136a78f70
c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[NH2;D1;+0:5]-[C:6]-[C:7]-[SH;D1;+0:8]>>[c:3]:[c:2](-[CH;D3;+0:1]1-[NH;D2;+0:5]-[C:6]-[C:7]-[S;H0;D2;+0:8]-1):[c:4]
91.4
[{"value": 91.4, "product": "C1(=CC=CC=C1)N1CCN(CC1)CCOC1=C(C=CC=C1)C1SCCN1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
2.21 g of sodium hydroxide are added to a solution of 5.75 g of cysteamine hydrochloride in 200 ml of ethanol, and a solution of 14.28 g of 2-[2-(4-phenylpiperazin-1-yl)ethyloxy]benzaldehyde in 100 ml of ethanol is added thereto. After the mixture is stirred at room temperature for 2 hours, the mixture is concentrated ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine.Aliphatic thiol
Secondary amine.Monosulfide
null
C1CSCN1
c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1.C1CSCN1
HO-
C(C)O
null
2
NCCS.O=Cc1ccccc1OCCN1CCN(c2ccccc2)CC1>C(C)O>c1ccc(N2CCN(CCOc3ccccc3C3NCCS3)CC2)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-09c579e755e541c2b07caf3e5cd2741f
COc1ncccc1C(=O)O>>COC(=O)c1cccnc1OC
S(=O)(Cl)Cl.COC1=NC=CC=C1C(=O)O.C(Cl)(Cl)(Cl)Cl>>COC1=NC=CC=C1C(=O)OC
[OH:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][n:9][c:10]1[O:11][CH3:12]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][n:9][c:10]1[O:11][CH3:12]
COc1ncccc1C(=O)O
COC(=O)c1cccnc1OC
null
null
null
Miscellaneous
Protection of carboxylic acid
56520e0abb4535dce9a663824ca803b71c2c0dd72dfd246317d953596a987bd2
2ccc7a30191c2c171b49e8a0217bee87430687dd0f567141eca025a75b7e3136
c1ccncc1
[#7;a:1]:[c:2]:[c:3]-[C:4](=[O;D1;H0:5])-[OH;D1;+0:6]>>[#7;a:1]:[c:2]:[c:3]-[C:4](=[O;D1;H0:5])-[O;H0;D2;+0:6]-[C;D1;H3:7]
null
[]
null
null
16
HOUR
Thionyl chloride (50 ml.) was added to 2-methoxypyridine-3-carboxylic acid (5 g.) in 50 ml. of carbon tetrachloride and the mixture refluxed for 2 hours. The reaction mixture was cooled, evaporated to solids and chased with multiple portions of fresh carbon tetrachloride. The resulting acid chloride hydrochloride was d...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ester
null
null
c1ccncc1
Other
null
null
16
COc1ncccc1C(=O)O>>COC(=O)c1cccnc1OC
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-29e55984d1184720b127405ae4f45163
CCN(CC)CC.COc1ncc(Cl)cc1C(=O)O>>COC(=O)c1cc(Cl)cnc1OC
ClC=1C=C(C(=NC1)OC)C(=O)O.C(C)N(CC)CC>>ClC=1C=C(C(=NC1)OC)C(=O)OC
CCN(CC)C[CH3:1].[OH:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([Cl:8])[cH:9][n:10][c:11]1[O:12][CH3:13]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([Cl:8])[cH:9][n:10][c:11]1[O:12][CH3:13]
CCN(CC)CC.COc1ncc(Cl)cc1C(=O)O
COC(=O)c1cc(Cl)cnc1OC
null
null
CO
Heteroatom Alkylation and Arylation
O-methylation
8ba133f06c4c0df103dfa8d83a3ae1c8f954a895eb15a5679d75dae29435b369
99f5e58a6f94b05681979232ec71674baa8e98488f497e30fe94f5f9a191f8d9
c1ccncc1
C-C-N(-C-C)-C-[CH3;D1;+0:1].[#7;a:2]:[c:3]:[c:4]-[C:5](=[O;D1;H0:6])-[OH;D1;+0:7]>>[#7;a:2]:[c:3]:[c:4]-[C:5](=[O;D1;H0:6])-[O;H0;D2;+0:7]-[CH3;D1;+0:1]
null
[]
null
null
null
null
By the procedure of Example 1, 5-chloro-2- methoxypyridine-3-carboxylic acid [Sarges et al., J. Med. Chem. 19, 709 (1976); 10 g.]was converted to its acid chloride, which was added in one portion to 150 ml. of methanol (slight exotherm), then made basic with triethylamine (approximately 1.1 equivalents). The reaction m...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Tertiary amine
Ester
null
null
c1ccncc1
Other
CO
null
null
CCN(CC)CC.COc1ncc(Cl)cc1C(=O)O>CO>COC(=O)c1cc(Cl)cnc1OC
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-610cc48c92ef4b2b91d458584a284769
CCOC(=O)C(O)c1cc(F)cc2cccnc12.[NH4+]>>NC(=O)C(O)c1cc(F)cc2cccnc12
FC=1C=C2C=CC=NC2=C(C1)C(C(=O)OCC)O.[OH-].[NH4+]>>FC=1C=C2C=CC=NC2=C(C1)C(C(=O)N)O
CCO[C:2](=[O:3])[CH:4]([OH:5])[c:6]1[cH:7][c:8]([F:9])[cH:10][c:11]2[cH:12][cH:13][cH:14][n:15][c:16]12.[NH4+:1]>>[NH2:1][C:2](=[O:3])[CH:4]([OH:5])[c:6]1[cH:7][c:8]([F:9])[cH:10][c:11]2[cH:12][cH:13][cH:14][n:15][c:16]12
CCOC(=O)C(O)c1cc(F)cc2cccnc12.[NH4+]
NC(=O)C(O)c1cc(F)cc2cccnc12
null
null
null
Acylation
OtherReaction
d5b10d4f469e7a196a3b04a6a9e159a7d90514b6df5b50c1197d4b1b774c04e1
adc0ef6f6c1340dd2dbab737c85bf17fc842769181c5db1a2b4f82b391b28f9f
c1ccc2ncccc2c1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[O;D1;H1:4])-[c:5]:[c:6]:[#7;a:7].[NH4+;D0:8]>>[#7;a:7]:[c:6]:[c:5]-[C:3](-[O;D1;H1:4])-[C;H0;D3;+0:1](-[NH2;D1;+0:8])=[O;D1;H0:2]
null
[]
null
null
null
null
Ethyl 2-(6-fluoro-8-quinolyl)-2-hydroxyacetate (1.1 g.) was refluxed for 10 minutes in 300 ml. of conc. ammonium hydroxide. The reaction mixture was cooled slightly, clarified by filtration and evaporated to solids. Trituration of the residue with 25 ml. of toluene gave the title product (860 mg., m.p. 169°-171° C.). C...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary amide
null
null
c1ccc2ncccc2c1
HO-
null
null
null
CCOC(=O)C(O)c1cc(F)cc2cccnc12.[NH4+]>>NC(=O)C(O)c1cc(F)cc2cccnc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-7eb2b9b7af004b369a2532d9aacf93e1
Cn1cccc1.O=C1NC(=O)C(=O)C(=O)N1>>Cn1cccc1C1(O)C(=O)NC(=O)NC1=O
O.N1C(=O)NC(=O)C(=O)C1=O.CN1C=CC=C1.Cl>>OC1(C(NC(NC1=O)=O)=O)C=1N(C=CC1)C
[CH3:1][n:2]1[cH:3][cH:4][cH:5][cH:6]1.[C:7]1(=[O:8])[C:9](=[O:10])[NH:11][C:12](=[O:13])[NH:14][C:15]1=[O:16]>>[CH3:1][n:2]1[cH:3][cH:4][cH:5][c:6]1[C:7]1([OH:8])[C:9](=[O:10])[NH:11][C:12](=[O:13])[NH:14][C:15]1=[O:16]
Cn1cccc1.O=C1NC(=O)C(=O)C(=O)N1
Cn1cccc1C1(O)C(=O)NC(=O)NC1=O
null
null
C(C)O
C-C Coupling
OtherReaction
a4c1a46ff012305b9e5a76446fe231f2c1c5f443a6c3c3af74a1ce06988920dd
454f67ba8644982dc9f605915a0f36178771eadaffb50d3f1e0f17f2b6fdeb10
O=C1NC(=O)C(c2ccc[nH]2)C(=O)N1
[C;D1;H3:1]-[#7;a:2]1:[c:3]:[c:4]:[c:5]:[cH;D2;+0:6]:1.[O;D1;H0:7]=[C:8]1-[#7:9]-[C:10](=[O;D1;H0:11])-[#7:12]-[C:13](=[O;D1;H0:14])-[C;H0;D3;+0:15]-1=[O;H0;D1;+0:16]>>[C;D1;H3:1]-[#7;a:2]1:[c:3]:[c:4]:[c:5]:[c;H0;D3;+0:6]:1-[C;H0;D4;+0:15]1(-[OH;D1;+0:16])-[C:13](=[O;D1;H0:14])-[#7:12]-[C:10](=[O;D1;H0:11])-[#7:9]-[C:...
65
[{"value": 5.0, "product": "OC1(C(NC(NC1=O)=O)=O)C=1N(C=CC1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 65.0, "product": "OC1(C(NC(NC1=O)=O)=O)C=1N(C=CC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
Alloxan hydrate (3.2 g., 0.02 mole) was dissolved in 50 ml. of ethanol by warming. 1-Methylpyrrole (1.6 g., 0.02 mole) was added and the mixture warmed for 5 minutes on a steam bath, while perfusing with hydrogen chloride. After standing at room temperature for 0.5 hour, the reaction mixture was evaporated to dryness a...
10.6084/m9.figshare.5104873.v1
null
Ketone
Tertiary alcohol
c1cc[nH]c1.C1CNCNC1
c1ccc[nH]1.C1CNCNC1
c1ccc[nH]1.C1CNCNC1
null
C(C)O
null
0.5
Cn1cccc1.O=C1NC(=O)C(=O)C(=O)N1>C(C)O>Cn1cccc1C1(O)C(=O)NC(=O)NC1=O
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-a21960842da8446c8bd423f866a07849
CCCCI.O=C1NC(=O)C(=O)C(=O)N1.c1cc[nH]c1>>CCCCn1cccc1C1(O)C(=O)NC(=O)NC1=O
Cl.N1C=CC=C1.[K].ICCCC.N1C(=O)NC(=O)C(=O)C1=O>>OC1(C(NC(NC1=O)=O)=O)C=1N(C=CC1)CCCC
I[CH2:4][CH2:3][CH2:2][CH3:1].[C:10]1(=[O:11])[C:12](=[O:13])[NH:14][C:15](=[O:16])[NH:17][C:18]1=[O:19].[nH:5]1[cH:6][cH:7][cH:8][cH:9]1>>[CH3:1][CH2:2][CH2:3][CH2:4][n:5]1[cH:6][cH:7][cH:8][c:9]1[C:10]1([OH:11])[C:12](=[O:13])[NH:14][C:15](=[O:16])[NH:17][C:18]1=[O:19]
CCCCI.O=C1NC(=O)C(=O)C(=O)N1.c1cc[nH]c1
CCCCn1cccc1C1(O)C(=O)NC(=O)NC1=O
null
null
O1CCCC1.C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
220be84d22102020d0dc799ad96f73134274c484ba4a32d0b1715b3d6dcb7ffb
589c80aa999ad622b2d6aa7f4cdee3f946916a025ab7700e5ceb34432777049f
O=C1NC(=O)C(c2ccc[nH]2)C(=O)N1
I-[CH2;D2;+0:1]-[C:2]-[C:3].[O;D1;H0:4]=[C:5]1-[#7:6]-[C:7](=[O;D1;H0:8])-[#7:9]-[C:10](=[O;D1;H0:11])-[C;H0;D3;+0:12]-1=[O;H0;D1;+0:13].[c:14]1:[c:15]:[c:16]:[cH;D2;+0:17]:[nH;D2;+0:18]:1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:18]1:[c:14]:[c:15]:[c:16]:[c;H0;D3;+0:17]:1-[C;H0;D4;+0:12]1(-[OH;D1;+0:13])-[C:5](=[O;D1;H0...
64.1
[{"value": 64.1, "product": "OC1(C(NC(NC1=O)=O)=O)C=1N(C=CC1)CCCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Potassium pyrrole (3.0 g., 0.03 mole), 1-iodobutane (9.2 g., 0.05 moles) and 10 ml. of tetrahydrofuran were combined and refluxed for 1.5 hours by which time the reaction mixture had become a thick mass. The reaction mixture was diluted with 30 ml. of water and extracted with 35 ml. of ether. The ether was backwashed w...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone
Tertiary alcohol
C1CNCNC1.c1cc[nH]c1
c1ccc[nH]1.C1CNCNC1
c1ccc[nH]1.C1CNCNC1
HI
O1CCCC1.C(C)O
null
null
CCCCI.O=C1NC(=O)C(=O)C(=O)N1.c1cc[nH]c1>O1CCCC1.C(C)O>CCCCn1cccc1C1(O)C(=O)NC(=O)NC1=O
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-95069968247c44b2ab51ec34ff101153
O=C1NC(=O)C(=O)C(=O)N1.c1ccc(-n2cccc2)cc1>>O=C1NC(=O)C(O)(c2cccn2-c2ccccc2)C(=O)N1
O.N1C(=O)NC(=O)C(=O)C1=O.C1(=CC=CC=C1)N1C=CC=C1.O.N1C(=O)NC(=O)C(=O)C1=O.Cl>>OC1(C(NC(NC1=O)=O)=O)C=1N(C=CC1)C1=CC=CC=C1
[O:1]=[C:2]1[NH:3][C:4](=[O:5])[C:6](=[O:7])[C:19](=[O:20])[NH:21]1.[cH:8]1[cH:9][cH:10][cH:11][n:12]1-[c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[C:6]([OH:7])([c:8]2[cH:9][cH:10][cH:11][n:12]2-[c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[C:19](=[O:20])[NH:21]1
O=C1NC(=O)C(=O)C(=O)N1.c1ccc(-n2cccc2)cc1
O=C1NC(=O)C(O)(c2cccn2-c2ccccc2)C(=O)N1
null
null
C(C)O
C-C Coupling
OtherReaction
a4c1a46ff012305b9e5a76446fe231f2c1c5f443a6c3c3af74a1ce06988920dd
454f67ba8644982dc9f605915a0f36178771eadaffb50d3f1e0f17f2b6fdeb10
O=C1NC(=O)C(c2cccn2-c2ccccc2)C(=O)N1
[O;D1;H0:1]=[C:2]1-[#7:3]-[C:4](=[O;D1;H0:5])-[C;H0;D3;+0:6](=[O;H0;D1;+0:7])-[C:8](=[O;D1;H0:9])-[#7:10]-1.[c:11]-[#7;a:12]1:[c:13]:[c:14]:[c:15]:[cH;D2;+0:16]:1>>[O;D1;H0:1]=[C:2]1-[#7:3]-[C:4](=[O;D1;H0:5])-[C;H0;D4;+0:6](-[OH;D1;+0:7])(-[c;H0;D3;+0:16]2:[c:15]:[c:14]:[c:13]:[#7;a:12]:2-[c:11])-[C:8](=[O;D1;H0:9])-[...
80.6
[{"value": 80.6, "product": "OC1(C(NC(NC1=O)=O)=O)C=1N(C=CC1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
1-Phenylpyrrole (1.4 g., 0.01 mole), alloxan hydrate (1.6 g., 0.01 mole) and 50 ml. of ethanol were combined and refluxed for 15 minutes. No reaction was noted by tlc. 1N Hydrochloric acid (10 ml., 0.01 mole) was added and the acidified mixture refluxed for 15 minutes. Incomplete reaction was noted by tlc. A second por...
10.6084/m9.figshare.5104873.v1
null
Ketone
Tertiary alcohol
C1CNCNC1.c1cc[nH]c1
C1CNCNC1.c1ccc[nH]1
C1CNCNC1.c1ccc[nH]1.c1ccccc1
null
C(C)O
null
null
O=C1NC(=O)C(=O)C(=O)N1.c1ccc(-n2cccc2)cc1>C(C)O>O=C1NC(=O)C(O)(c2cccn2-c2ccccc2)C(=O)N1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-cea0023b4b3542e7b1758742907c3ede
Brc1ccc2[nH]ccc2c1.O=C1NC(=O)C(=O)C(=O)N1>>O=C1NC(=O)C(O)(c2c[nH]c3ccc(Br)cc23)C(=O)N1
O.N1C(=O)NC(=O)C(=O)C1=O.BrC=1C=C2C=CNC2=CC1.Cl>>OC1(C(NC(NC1=O)=O)=O)C1=CNC2=CC=C(C=C12)Br
[cH:8]1[cH:9][nH:10][c:11]2[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]12.[O:1]=[C:2]1[NH:3][C:4](=[O:5])[C:6](=[O:7])[C:18](=[O:19])[NH:20]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[C:6]([OH:7])([c:8]2[cH:9][nH:10][c:11]3[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]23)[C:18](=[O:19])[NH:20]1
Brc1ccc2[nH]ccc2c1.O=C1NC(=O)C(=O)C(=O)N1
O=C1NC(=O)C(O)(c2c[nH]c3ccc(Br)cc23)C(=O)N1
null
null
C(C)O
C-C Coupling
OtherReaction
7c628cde874505d70066b03c9296773cfbcdc40c0f4563afcdc554abdd3b32c8
454f67ba8644982dc9f605915a0f36178771eadaffb50d3f1e0f17f2b6fdeb10
O=C1NC(=O)C(c2c[nH]c3ccccc23)C(=O)N1
[O;D1;H0:1]=[C:2]1-[#7:3]-[C:4](=[O;D1;H0:5])-[#7:6]-[C:7](=[O;D1;H0:8])-[C;H0;D3;+0:9]-1=[O;H0;D1;+0:10].[c:11]:[c:12]1:[#7;a:13]:[c:14]:[cH;D2;+0:15]:[c:16]:1:[c:17]>>[O;D1;H0:1]=[C:2]1-[#7:3]-[C:4](=[O;D1;H0:5])-[#7:6]-[C:7](=[O;D1;H0:8])-[C;H0;D4;+0:9]-1(-[OH;D1;+0:10])-[c;H0;D3;+0:15]1:[c:14]:[#7;a:13]:[c:12](:[c:...
93.8
[{"value": 93.8, "product": "OC1(C(NC(NC1=O)=O)=O)C1=CNC2=CC=C(C=C12)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
Alloxan hydrate (1.6 g., 0.01 mole) was dissolved in 40 ml. of ethanol by heating. 5-Bromoindole (1.96 g., 0.01 mole) was added and heating near reflux continued for 15 minutes. Tlc did not indicate that reaction had occured. 1N Hydrochloric acid (10 ml.) was then added while maintaining the reaction near reflux. After...
10.6084/m9.figshare.5104873.v1
null
Ketone
Tertiary alcohol
c1ccc2[nH]ccc2c1.C1CNCNC1
C1CNCNC1.c1ccc2[nH]ccc2c1
C1CNCNC1.c1ccc2[nH]ccc2c1
null
C(C)O
null
0.25
Brc1ccc2[nH]ccc2c1.O=C1NC(=O)C(=O)C(=O)N1>C(C)O>O=C1NC(=O)C(O)(c2c[nH]c3ccc(Br)cc23)C(=O)N1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-8a9b468035a9458e96d4a4f5d9967faa
O=C1NC(=O)C(=O)C(=O)N1.c1ccc2scnc2c1>>O=C1NC(=O)C(O)(c2nc3ccccc3s2)C(=O)N1
S1C=NC2=C1C=CC=C2.N1C(=O)NC(=O)C(=O)C1=O>>OC1(C(NC(NC1=O)=O)=O)C=1SC2=C(N1)C=CC=C2
[O:1]=[C:2]1[NH:3][C:4](=[O:5])[C:6](=[O:7])[C:17](=[O:18])[NH:19]1.[cH:8]1[n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[s:16]1>>[O:1]=[C:2]1[NH:3][C:4](=[O:5])[C:6]([OH:7])([c:8]2[n:9][c:10]3[cH:11][cH:12][cH:13][cH:14][c:15]3[s:16]2)[C:17](=[O:18])[NH:19]1
O=C1NC(=O)C(=O)C(=O)N1.c1ccc2scnc2c1
O=C1NC(=O)C(O)(c2nc3ccccc3s2)C(=O)N1
null
null
null
C-C Coupling
OtherReaction
d9aa83a883a197037fdd31c3d054c7bd874ee758a6aa8bcdd6296a903ccc5f38
454f67ba8644982dc9f605915a0f36178771eadaffb50d3f1e0f17f2b6fdeb10
O=C1NC(=O)C(c2nc3ccccc3s2)C(=O)N1
[#16;a:1]1:[c:2]:[c:3]:[#7;a:4]:[cH;D2;+0:5]:1.[O;D1;H0:6]=[C:7]1-[#7:8]-[C:9](=[O;D1;H0:10])-[#7:11]-[C:12](=[O;D1;H0:13])-[C;H0;D3;+0:14]-1=[O;H0;D1;+0:15]>>[O;D1;H0:6]=[C:7]1-[#7:8]-[C:9](=[O;D1;H0:10])-[#7:11]-[C:12](=[O;D1;H0:13])-[C;H0;D4;+0:14]-1(-[OH;D1;+0:15])-[c;H0;D3;+0:5]1:[#16;a:1]:[c:2]:[c:3]:[#7;a:4]:1
null
[]
null
null
null
null
By the procedure of Example 38, benzthiazole (2.7 g., 0.02 moles) was converted to its 2-lithio derivative and then reacted with anhydrous alloxan to yield title product, initially isolated as an oil. The latter was crystallized from ether-hexane [2.2 g.; Rf 0.55 (1:1 ethyl acetate:hexane/5% acetic acid)]. Conditions: ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Tertiary alcohol
C1CNCNC1.c1ccc2scnc2c1
C1CNCNC1.c1ccc2scnc2c1
C1CNCNC1.c1ccc2scnc2c1
null
null
null
null
O=C1NC(=O)C(=O)C(=O)N1.c1ccc2scnc2c1>>O=C1NC(=O)C(O)(c2nc3ccccc3s2)C(=O)N1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-cc968f431e0a486dbfd6bbc5f8b29349
C[O-].O=C(O)c1cccnc1Cl>>COc1ncccc1C(=O)O
ClC1=NC=CC=C1C(=O)O.C[O-].[Na+]>>COC1=NC=CC=C1C(=O)O
[CH3:1][O-:2].Cl[c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[C:9](=[O:10])[OH:11]>>[CH3:1][O:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[C:9](=[O:10])[OH:11]
C[O-].O=C(O)c1cccnc1Cl
COc1ncccc1C(=O)O
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
600484490705932a09b3fac6538a42c6f3fc156ab44a4ea0bbd020dd3eafd6ff
51fd03eb6a688046e417b9ed09ea0e72062396d005af1318b9b5f376a97da959
c1ccncc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[C:5](=[O;D1;H0:6])-[O;D1;H1:7]):[c:8].[C;D1;H3:9]-[O-;H0;D1:10]>>[C;D1;H3:9]-[O;H0;D2;+0:10]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[C:5](=[O;D1;H0:6])-[O;D1;H1:7]):[c:8]
null
[]
110
CELSIUS
30
MINUTE
A stainless steel stirred autoclave was charged sequentially with methanol (2.8 1.), sodium methoxide (259 g.) (in portions, keeping the temperature less than 35° C.), and 2-chloro-3-pyridinecarboxylic acid (190 g.). The autoclave was sealed and the reaction mixture heated at 110° C. (50 psig) for 48 hours. The reactio...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Ether
c1ccncc1
c1ccncc1
c1ccncc1
Other
CO
110
0.5
C[O-].O=C(O)c1cccnc1Cl>CO>COc1ncccc1C(=O)O
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-3792b8f5158c4708b58669947fcd21e1
CCOC(=O)C(=O)OCC.Clc1cc(Br)c2ncccc2c1>>CCOC(=O)C(=O)c1cc(Cl)cc2cccnc12
C(CCC)[Li].BrC=1C=C(C=C2C=CC=NC12)Cl.C(C(=O)OCC)(=O)OCC>>ClC=1C=C2C=CC=NC2=C(C1)C(C(=O)OCC)=O
CCO[C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])=[O:7].Br[c:8]1[cH:9][c:10]([Cl:11])[cH:12][c:13]2[cH:14][cH:15][cH:16][n:17][c:18]12>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6](=[O:7])[c:8]1[cH:9][c:10]([Cl:11])[cH:12][c:13]2[cH:14][cH:15][cH:16][n:17][c:18]12
CCOC(=O)C(=O)OCC.Clc1cc(Br)c2ncccc2c1
CCOC(=O)C(=O)c1cc(Cl)cc2cccnc12
null
null
O1CCCC1
C-C Coupling
Ester and halide to ketone
3dbcbbaf463d6c40c5052a565558cc24c1b64e60a3b9034219110c98b23faabc
dd03ca4e617545414fae7e22c410ecd4f78e4fd10d5a86bce7e36a4a1d0f1e9d
c1ccc2ncccc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].C-C-O-[C;H0;D3;+0:8](=[O;D1;H0:9])-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]>>[C:13]-[#8:12]-[C:10](=[O;D1;H0:11])-[C;H0;D3;+0:8](=[O;D1;H0:9])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]
null
[]
0
CELSIUS
30
MINUTE
8-Bromo-6-chloroquinoline [J. Het. Chem. 6, pp. 243-245 (1969); 6 g., 0.025 mole]in 50 ml. of tetrahydrofuran was added dropwise over a 10 minute period to a mixture of butyl lithium (2.3 M in hexane, 12.2 ml., 0.028 mole) and 40 ml. of tetrahydrofuran held at -70° C. After an additional 30 minutes at this temperature,...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ester.Ester
Ketone
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HBr
O1CCCC1
0
0.5
CCOC(=O)C(=O)OCC.Clc1cc(Br)c2ncccc2c1>O1CCCC1>CCOC(=O)C(=O)c1cc(Cl)cc2cccnc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-88edf4562ff1434b84869e91d827f11b
O.Oc1ccc2ncccc2c1>>O=Cc1c(O)ccc2ncccc12
C(Cl)(Cl)Cl.[OH-].[Na+].O.C(Cl)(Cl)Cl.OC=1C=C2C=CC=NC2=CC1>>OC1=C(C=2C=CC=NC2C=C1)C=O
[OH2:1].[cH:3]1[c:4]([OH:5])[cH:6][cH:7][c:8]2[n:9][cH:10][cH:11][cH:12][c:13]12>>[O:1]=[CH:2][c:3]1[c:4]([OH:5])[cH:6][cH:7][c:8]2[n:9][cH:10][cH:11][cH:12][c:13]12
O.Oc1ccc2ncccc2c1
O=Cc1c(O)ccc2ncccc12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
b448291d461d839ae70a6a1ab399b0e7d61d1ad82e7df41b54a00ef11e9f4879
be117abed4a0a0378ea43d3a5c1ccf903b86823ade7e92fcb09d68743e45d19a
c1ccc2ncccc2c1
[O;D1;H1:1]-[c:2]1:[c:3]:[c:4]:[c:5](:[#7;a:6]:[c:7]):[c:8](:[c:9]):[cH;D2;+0:10]:1.[OH2;D0;+0:11]>>[O;D1;H1:1]-[c:2]1:[c:3]:[c:4]:[c:5](:[#7;a:6]:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:10]:1-[C:12]=[O;H0;D1;+0:11]
null
[]
90
CELSIUS
6
HOUR
Sodium hydroxide (25 g.) was dissolved in 35 ml. of water with cooling, 6-hydroxyquinoline (5 g.) in 15 ml. of chloroform was added and the reaction mixture heated to reflux (about 90° C.) for 12 hours, during which two further 15 ml. portions of chloroform were added - one after 2 hours and the other after 6 hours. Th...
10.6084/m9.figshare.5104873.v1
null
null
Aldehyde
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
Other
null
90
6
O.Oc1ccc2ncccc2c1>>O=Cc1c(O)ccc2ncccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-49296d2357364b18b0d51fff59527d15
O=C(O)c1cc2ccc(Cl)cc2o1>>O=C(O)c1cc2cc(Cl)ccc2o1
ClC=1C=CC=C(C1C=O)O.FC1=CC2=C(OC(=C2)C(=O)O)C=C1.ClC=1C=CC2=C(OC(=C2)C(=O)O)C1>>ClC1=CC2=C(OC(=C2)C(=O)O)C=C1
[O:1]=[C:2]([OH:3])[c:4]1[cH:5][c:12]2[c:6]([cH:7][c:8]([Cl:9])[cH:10][cH:11]2)[o:13]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][c:6]2[cH:7][c:8]([Cl:9])[cH:10][cH:11][c:12]2[o:13]1
O=C(O)c1cc2ccc(Cl)cc2o1
O=C(O)c1cc2cc(Cl)ccc2o1
null
null
null
Miscellaneous
OtherReaction
6919e7905146bdc0c46835415551780572928af110d80d2e3da217b6e11a99fc
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc2occc2c1
[O;D1;H0:1]=[C:2](-[O;D1;H1:3])-[c:4]1:[cH;D2;+0:5]:[c;H0;D3;+0:6]2:[c:7]:[c:8]:[c:9]:[c:10]:[c;H0;D3;+0:11]:2:[o;H0;D2;+0:12]:1>>[O;D1;H0:1]=[C:2](-[O;D1;H1:3])-[c:4]1:[cH;D2;+0:5]:[c;H0;D3;+0:11]2:[c:10]:[c:9]:[c:8]:[c:7]:[c;H0;D3;+0:6]:2:[o;H0;D2;+0:12]:1
null
[]
null
null
null
null
By the same procedure, 5-fluorosalicyaldehyde and 6-chlorosalicylaldehyde are converted, respectively, to 5-fluorobenzo[b]furan-2-carboxylic acid and 6-chlorobenzo[b]furan-2-carboxylic acid. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2occc2c1
c1ccc2occc2c1
c1ccc2occc2c1
null
null
null
null
O=C(O)c1cc2ccc(Cl)cc2o1>>O=C(O)c1cc2cc(Cl)ccc2o1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-75f04b9b625845f494cd468f75c57ffe
Cc1c(Cl)ccc2cccnc12.O=C1CCC(=O)N1Br>>Clc1ccc2cccnc2c1CBr
ClC1=CC=C2C=CC=NC2=C1C.BrN1C(CCC1=O)=O>>ClC1=CC=C2C=CC=NC2=C1CBr
[Cl:1][c:2]1[cH:3][cH:4][c:5]2[cH:6][cH:7][cH:8][n:9][c:10]2[c:11]1[CH3:12].O=C1CCC(=O)N1[Br:13]>>[Cl:1][c:2]1[cH:3][cH:4][c:5]2[cH:6][cH:7][cH:8][n:9][c:10]2[c:11]1[CH2:12][Br:13]
Cc1c(Cl)ccc2cccnc12.O=C1CCC(=O)N1Br
Clc1ccc2cccnc2c1CBr
null
null
C1=CC=CC=C1
Functional Group Interconversion
Wohl-Ziegler bromination benzyl primary
45c0aca0d63a96f0092e6dded9c888827eaf6379dac179e1cefc99293896300a
08f5e7e34d3f321cce3e85421b38226d6240cca0939494ae61032d4f8405cf22
c1ccc2ncccc2c1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5](:[c:6]):[#7;a:7]:[c:8]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5](:[c:6]):[#7;a:7]:[c:8]
null
[]
null
null
null
null
7-Chloro-8-methylquinoline (1 g.) [Bradford et al., J. Chem Soc., p. 437 (1947)]is dissolved in 20 ml. of benzene and brominated with one equivalent of N-bromosuccinimide in the presence of catalytic amounts of peroxide. The product, 7-chloro-8-(bromomethyl)quinoline is isolated by evaporation Conditions: See reaction....
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Primary halide
C1CCNC1
null
c1ccc2ncccc2c1
HO-
C1=CC=CC=C1
null
null
Cc1c(Cl)ccc2cccnc12.O=C1CCC(=O)N1Br>C1=CC=CC=C1>Clc1ccc2cccnc2c1CBr
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-5c24f2117d6a447bb1c6127ce54bb126
BrBr.CC(=O)C1Cc2ccccc2C1>>O=C(CBr)C1Cc2ccccc2C1
BrBr.BrBr.C1C(CC2=CC=CC=C12)C(C)=O.BrBr>>BrCC(=O)C1CC2=CC=CC=C2C1
Br[Br:4].[O:1]=[C:2]([CH3:3])[CH:5]1[CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[CH2:13]1>>[O:1]=[C:2]([CH2:3][Br:4])[CH:5]1[CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[CH2:13]1
BrBr.CC(=O)C1Cc2ccccc2C1
O=C(CBr)C1Cc2ccccc2C1
null
null
CCOCC
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccc2c(c1)CCC2
Br-[Br;H0;D1;+0:1].[C:2]-[C:3](-[CH3;D1;+0:4])=[O;D1;H0:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:4]-[C:3](-[C:2])=[O;D1;H0:5]
null
[]
null
null
null
null
Bromine (6.8 g) is slowly added to a stirred solution of 1-(2,3-dihydro-1H-inden-2-yl)ethanone (6.8 g) in 200 ml of dry ether, while keeping the temperature at +10° C. The rate of the addition of bromine is controlled so that the colour due to one added portion of bromine has been discharged before another portion is a...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccc2c(c1)CCC2
HBr
CCOCC
null
null
BrBr.CC(=O)C1Cc2ccccc2C1>CCOCC>O=C(CBr)C1Cc2ccccc2C1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-831b47ccaa75402fb592e9fa15e798c2
BrBr.CC(=O)c1cc2ccccc2o1>>O=C(CBr)c1cc2ccccc2o1
CC(=O)C=1OC2=C(C1)C=CC=C2.BrBr>>O1C(=CC2=C1C=CC=C2)C(CBr)=O
Br[Br:4].[O:1]=[C:2]([CH3:3])[c:5]1[cH:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[o:13]1>>[O:1]=[C:2]([CH2:3][Br:4])[c:5]1[cH:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[o:13]1
BrBr.CC(=O)c1cc2ccccc2o1
O=C(CBr)c1cc2ccccc2o1
null
null
C(Cl)Cl
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccc2occc2c1
Br-[Br;H0;D1;+0:1].[#8;a:2]:[c:3]-[C:4](-[CH3;D1;+0:5])=[O;D1;H0:6]>>[#8;a:2]:[c:3]-[C:4](=[O;D1;H0:6])-[CH2;D2;+0:5]-[Br;H0;D1;+0:1]
null
[]
null
null
2
HOUR
Benzofuran-2-yl methyl ketone (20 g) is dissolved in 100 ml of methylene chloride and 3.2 ml of bromine in methylene chloride is added at 5°-10° C. Then the reaction mixture is stirred at +15° C. for 2 hours. Then it is washed with water, with diluted sodium bicarbonate solution and again with water. The organic phase ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccc2occc2c1
HBr
C(Cl)Cl
null
2
BrBr.CC(=O)c1cc2ccccc2o1>C(Cl)Cl>O=C(CBr)c1cc2ccccc2o1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-5a05f21af04347eba8fca34c13fc77a3
C[C@@H]1c2ccccc2C[C@@H]1C(=O)O.O=S(Cl)Cl>>C[C@@H]1c2ccccc2C[C@@H]1C(=O)Cl
C[C@H]1[C@H](CC2=CC=CC=C12)C(=O)O.S(=O)(Cl)Cl>>C[C@H]1[C@H](CC2=CC=CC=C12)C(=O)Cl
O[C:11]([C@@H:10]1[C@H:2]([CH3:1])[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9]1)=[O:12].O=S(Cl)[Cl:13]>>[CH3:1][C@@H:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][C@@H:10]1[C:11](=[O:12])[Cl:13]
C[C@@H]1c2ccccc2C[C@@H]1C(=O)O.O=S(Cl)Cl
C[C@@H]1c2ccccc2C[C@@H]1C(=O)Cl
null
null
null
Functional Group Interconversion
Alcohol to chloride_SOCl2
c301c14a9dcd0670d52e8b77396cbe7fd8edeedd757bc43f4162ade1fc52fc93
787f545db5dc0b29dde55b5fbed7db8625b8055f49327f97ed4d83cc47c3af1d
c1ccc2c(c1)CCC2
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](-[C:5])-[C:6]>>[C:5]-[C:4](-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3])-[C:6]
null
[]
null
null
null
null
cis-2,3-Dihydro-1-methyl-1H-indene-2-carboxylic acid (52.6 g) is converted to its acid chloride by treatment with thionyl chloride (130 ml). Excess thionyl chloride is distilled off and the acid chloride is distilled, b.p. 86°-89° C./0.45 mmHg. The yield is 47.9 g, 83%. Conditions: See reaction.notes.procedure_details....
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Acyl halide
null
null
c1ccc2c(c1)CCC2
HCl
null
null
null
C[C@@H]1c2ccccc2C[C@@H]1C(=O)O.O=S(Cl)Cl>>C[C@@H]1c2ccccc2C[C@@H]1C(=O)Cl
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-0c8bd1726a624b558cf9760fcb686e24
C[C@@H]1c2ccccc2C[C@@H]1C(=O)Cl>>CC(=O)[C@H]1Cc2ccccc2[C@H]1C
C[C@H]1[C@H](CC2=CC=CC=C12)C(=O)Cl.CCOCC.S(O)(O)(=O)=O>>C[C@H]1[C@H](CC2=CC=CC=C12)C(C)=O
Cl[C:2](=[O:3])[C@H:4]1[CH2:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]2[C@H:12]1[CH3:13]>>[CH3:1][C:2](=[O:3])[C@H:4]1[CH2:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]2[C@H:12]1[CH3:13]
C[C@@H]1c2ccccc2C[C@@H]1C(=O)Cl
CC(=O)[C@H]1Cc2ccccc2[C@H]1C
null
null
null
Functional Group Interconversion
OtherReaction
4e817a5ec78c6c2a6f84aedb26a0e8811be631b20b7d07ec665e1c596667189c
f6f1db2fb6b7641a5cc9b525399565f319b23dea2171a8a2e15ad3fed644bcab
c1ccc2c(c1)CCC2
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5]>>[C:4]-[C:3](-[C;H0;D3;+0:1](-[C;D1;H3:6])=[O;D1;H0:2])-[C:5]
92
[{"value": 92.0, "product": "C[C@H]1[C@H](CC2=CC=CC=C12)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
cis-1-(2,3-Dihydro-1-methyl-1H-inden-2-yl)ethanone is prepared by the treatment of cis-2,3-dihydro-1-methyl-1H-indene-2-carboxylic acid chloride with ethoxymagnesiummalonic acid ethyl ester in dry ether and thereafter by the treatment of sulfuric acid according to the publication (Reynolds G. A. and Hauser, C. B., Org....
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Ketone
null
null
c1ccc2c(c1)CCC2
null
null
null
null
C[C@@H]1c2ccccc2C[C@@H]1C(=O)Cl>>CC(=O)[C@H]1Cc2ccccc2[C@H]1C
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-8626b45b275c4e28bae2be02833668e2
CC(=O)C1(Br)Cc2ccccc2C1C.C[C@@H]1c2ccccc2C[C@@H]1C(=O)CBr>>CC1c2ccccc2CC1(Br)C(=O)CBr
BrCC(=O)[C@@H]1[C@@H](C2=CC=CC=C2C1)C.BrBr.BrBr.C[C@H]1[C@H](CC2=CC=CC=C12)C(C)=O.BrC1(C(C2=CC=CC=C2C1)C)C(C)=O>>BrCC(=O)C1(C(C2=CC=CC=C2C1)C)Br
[CH3:1][CH:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][C:10]1([Br:11])[C:12](=[O:13])[CH3:14].C[C@@H]1c2ccccc2C[C@@H]1C(=O)C[Br:15]>>[CH3:1][CH:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][C:10]1([Br:11])[C:12](=[O:13])[CH2:14][Br:15]
CC(=O)C1(Br)Cc2ccccc2C1C.C[C@@H]1c2ccccc2C[C@@H]1C(=O)CBr
CC1c2ccccc2CC1(Br)C(=O)CBr
null
null
C(Cl)Cl
Functional Group Interconversion
Bromination
02a16af959daa02973ed686e9293b78635f4a648224716be7230eeabbda243ff
e75d27ba56381d95767cb1073c9e300bbe7fb0cf89d3bae527844cbd5245737b
c1ccc2c(c1)CCC2
C-[C@H]1-[C@H](-C(=O)-C-[Br;H0;D1;+0:1])-C-c2:c:c:c:c:c:2-1.[C:2]-[C:3](-[CH3;D1;+0:4])=[O;D1;H0:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:4]-[C:3](-[C:2])=[O;D1;H0:5]
null
[]
null
null
null
null
Bromine in methylene chloride is slowly added to a stirred solution of cis-1-(2,3-dihydro-1-methyl-1H-inden-2-yl)ethanone (34.8 g) in methylene chloride (835 ml), while keeping the temperature at +10° C. The reaction is followed by GLC. The first products are the isomers of 1-(2-bromo-2,3-dihydro-1-methyl-1H-inden-2-yl...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Ketone
Primary halide
c1ccc2c(c1)CCC2
null
c1ccc2c(c1)CCC2
HO-
C(Cl)Cl
null
null
CC(=O)C1(Br)Cc2ccccc2C1C.C[C@@H]1c2ccccc2C[C@@H]1C(=O)CBr>C(Cl)Cl>CC1c2ccccc2CC1(Br)C(=O)CBr
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-7ea4f8fc554c4262acbd33d788d8a118
Cc1ccc2c(c1)C(C)C(C(=O)O)=C2>>CC1=C(C(=O)O)Cc2ccc(C)cc21
CC1C(=CC2=CC=C(C=C12)C)C(=O)O.C(C)OC(C(CC1=CC=C(C=C1)C)C(C)=O)=O.S(O)(O)(=O)=O>>CC1=C(CC2=CC=C(C=C12)C)C(=O)O
[CH3:1][CH:2]1[C:3]([C:4](=[O:5])[OH:6])=[CH:7][c:8]2[cH:9][cH:10][c:11]([CH3:12])[cH:13][c:14]21>>[CH3:1][C:2]1=[C:3]([C:4](=[O:5])[OH:6])[CH2:7][c:8]2[cH:9][cH:10][c:11]([CH3:12])[cH:13][c:14]21
Cc1ccc2c(c1)C(C)C(C(=O)O)=C2
CC1=C(C(=O)O)Cc2ccc(C)cc21
null
null
null
Miscellaneous
OtherReaction
a7595144baf9ed16d69ef1cd82fd2cf6644c447d3eba2ace35dfdcca34f79f0f
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
C1=Cc2ccccc2C1
[C;D1;H3:1]-[CH;D3;+0:2]1-[C;H0;D3;+0:3](-[C:4](=[O;D1;H0:5])-[O;D1;H1:6])=[CH;D2;+0:7]-[c:8](:[c:9]):[c:10]-1:[c:11]>>[C;D1;H3:1]-[C;H0;D3;+0:2]1=[C;H0;D3;+0:3](-[C:4](=[O;D1;H0:5])-[O;D1;H1:6])-[CH2;D2;+0:7]-[c:8](:[c:9]):[c:10]-1:[c:11]
59
[{"value": 59.0, "product": "CC1=C(CC2=CC=C(C=C12)C)C(=O)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The 1,6-dimethyl-indene-2-carboxylic acid can be prepared by the treatment of α-acetyl-4-methylbenzenepropanoic acid ethyl ester with sulfuric acid (Shadbolt, R. S., J. Chem. Soc. (C), (1970) 920). Recrystallization from ethanol, m.p. 174°-182° C. Yield 59%. Conditions: See reaction.notes.procedure_details. Workup: Rec...
10.6084/m9.figshare.5104873.v1
null
null
null
C1=Cc2ccccc2C1
C1=Cc2ccccc2C1
C1=Cc2ccccc2C1
null
null
null
null
Cc1ccc2c(c1)C(C)C(C(=O)O)=C2>>CC1=C(C(=O)O)Cc2ccc(C)cc21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-87df338463cf4ff9b0aae301b7d4b2ce
CC1=C(C(=O)O)Cc2ccc(C)cc21.O=S(Cl)Cl>>CC1=C(C(=O)Cl)Cc2ccc(C)cc21
CC1=C(CC2=CC=C(C=C12)C)C(=O)O.S(=O)(Cl)Cl>>CC1=C(CC2=CC=C(C=C12)C)C(=O)Cl
O[C:4]([C:3]1=[C:2]([CH3:1])[c:14]2[c:8]([cH:9][cH:10][c:11]([CH3:12])[cH:13]2)[CH2:7]1)=[O:5].O=S(Cl)[Cl:6]>>[CH3:1][C:2]1=[C:3]([C:4](=[O:5])[Cl:6])[CH2:7][c:8]2[cH:9][cH:10][c:11]([CH3:12])[cH:13][c:14]21
CC1=C(C(=O)O)Cc2ccc(C)cc21.O=S(Cl)Cl
CC1=C(C(=O)Cl)Cc2ccc(C)cc21
null
null
null
Functional Group Interconversion
Alcohol to chloride_SOCl2
c301c14a9dcd0670d52e8b77396cbe7fd8edeedd757bc43f4162ade1fc52fc93
787f545db5dc0b29dde55b5fbed7db8625b8055f49327f97ed4d83cc47c3af1d
C1=Cc2ccccc2C1
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](=[C:5](-[C;D1;H3:6])-[c:7])-[C:8]>>[C:8]-[C:4](-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3])=[C:5](-[C;D1;H3:6])-[c:7]
null
[]
null
null
null
null
3,5-Dimethyl-indene-2-carboxylic acid (37.3 g) is converted to its acid chloride by treatment with thionyl chloride (580 ml). Excess thionyl chloride is distilled off. Yield 40.5 g, 99%. Conditions: See reaction.notes.procedure_details. Workup: Excess thionyl chloride is distilled off
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Acyl halide
null
null
C1=Cc2ccccc2C1
HCl
null
null
null
CC1=C(C(=O)O)Cc2ccc(C)cc21.O=S(Cl)Cl>>CC1=C(C(=O)Cl)Cc2ccc(C)cc21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-ab458a1226a44a2ab6a4a788fe7dda8f
CC(=O)[C@H]1Cc2ccccc2[C@H]1C>>CC(=O)C1=C(C)c2cc(C)ccc2C1
CCOCC.C[C@H]1[C@H](CC2=CC=CC=C12)C(C)=O>>CC1=C(CC2=CC=C(C=C12)C)C(C)=O
[CH3:1][C:2](=[O:3])[C@@H:4]1[C@H:5]([CH3:6])[c:7]2[cH:8][cH:9][cH:11][cH:12][c:13]2[CH2:14]1>>[CH3:1][C:2](=[O:3])[C:4]1=[C:5]([CH3:6])[c:7]2[cH:8][c:9]([CH3:10])[cH:11][cH:12][c:13]2[CH2:14]1
CC(=O)[C@H]1Cc2ccccc2[C@H]1C
CC(=O)C1=C(C)c2cc(C)ccc2C1
null
null
O1CCCC1
Miscellaneous
OtherReaction
1428ddf264ea39b942080957ee8b8fd9368b1a5c11740576518d93da93c2dd22
f394080031812a9c0cde55fa330311dfe42bea38dbdf0b4621700859838ffa32
C1=Cc2ccccc2C1
[C;D1;H3:1]-[C:2](=[O;D1;H0:3])-[C@H;D3;+0:4]1-[C:5]-[c:6]2:[c:7]:[c:8]:[cH;D2;+0:9]:[c:10]:[c:11]:2-[C@H;D3;+0:12]-1-[C;D1;H3:13]>>[C;D1;H3:14]-[c;H0;D3;+0:9]1:[c:8]:[c:7]:[c:6]2:[c:11](:[c:10]:1)-[C;H0;D3;+0:12](-[C;D1;H3:13])=[C;H0;D3;+0:4](-[C:2](-[C;D1;H3:1])=[O;D1;H0:3])-[C:5]-2
84
[{"value": 84.0, "product": "CC1=C(CC2=CC=C(C=C12)C)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
1-(3,5-Dimethyl-inden-2-yl)ethanone is prepared by the same procedure as cis-1-(2,3-dihydro-1-methyl-1H-inden-2-yl)ethanone in Example 4b. A mixture of dry ether and tetrahydrofuran is used as solvent. Yield 84%. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone
Ketone
c1ccc2c(c1)CCC2
C1=Cc2ccccc2C1
C1=Cc2ccccc2C1
Other
O1CCCC1
null
null
CC(=O)[C@H]1Cc2ccccc2[C@H]1C>O1CCCC1>CC(=O)C1=C(C)c2cc(C)ccc2C1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-87ac3ca1a6a44205a81100de76b418af
BrBr.CC(=O)C1=C(C)c2cc(C)ccc2C1>>Cc1ccc2c(c1)C(C)C(C(=O)CBr)=C2
BrBr.CC1=C(CC2=CC=C(C=C12)C)C(C)=O>>BrCC(=O)C=1C(C2=CC(=CC=C2C1)C)C
Br[Br:14].[CH3:1][c:2]1[cH:3][cH:4][c:5]2[c:6]([cH:7]1)[C:8]([CH3:9])=[C:10]([C:11](=[O:12])[CH3:13])[CH2:15]2>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[c:6]([cH:7]1)[CH:8]([CH3:9])[C:10]([C:11](=[O:12])[CH2:13][Br:14])=[CH:15]2
BrBr.CC(=O)C1=C(C)c2cc(C)ccc2C1
Cc1ccc2c(c1)C(C)C(C(=O)CBr)=C2
null
null
CCOCC
Functional Group Interconversion
OtherReaction
63511e44f801465d677c29ade9e74644ea21572114dd81cfb6199c9456c67fab
eb663644836e52c1f41296c3f69eb0e554d5dc7739685ba436d901c3ef080ab9
C1=Cc2ccccc2C1
Br-[Br;H0;D1;+0:1].[C;D1;H3:2]-[C;H0;D3;+0:3]1=[C;H0;D3;+0:4](-[C:5](-[CH3;D1;+0:6])=[O;D1;H0:7])-[CH2;D2;+0:8]-[c:9](:[c:10]):[c:11]-1:[c:12]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:6]-[C:5](=[O;D1;H0:7])-[C;H0;D3;+0:4]1=[CH;D2;+0:8]-[c:9](:[c:10]):[c:11](:[c:12])-[CH;D3;+0:3]-1-[C;D1;H3:2]
59.5
[{"value": 59.0, "product": "BrCC(=O)C=1C(C2=CC(=CC=C2C1)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 59.5, "product": "BrCC(=O)C=1C(C2=CC(=CC=C2C1)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Bromine (2.80 g) is added to 1-(3,5-dimethyl-inden-2-yl)ethanone (3.00 g) in dry ether (30 ml), while keeping the temperature at +10° C. The mixture is extracted with water, several times with the diluted NaHCO3 solution, again with water, dried and evaporated under reduced pressure to afford the product (2.54 g, 59%)....
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide.Ketone
C1=Cc2ccccc2C1
C1=Cc2ccccc2C1
C1=Cc2ccccc2C1
HBr
CCOCC
null
null
BrBr.CC(=O)C1=C(C)c2cc(C)ccc2C1>CCOCC>Cc1ccc2c(c1)C(C)C(C(=O)CBr)=C2
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-444387114cd14a4393559ebdbf1888ba
Cc1cccc2c1C=C(C(=O)O)C2C.O=S(Cl)Cl>>Cc1cccc2c1C=C(C(=O)Cl)C2C
CC1C(=CC2=C(C=CC=C12)C)C(=O)O.S(=O)(Cl)Cl>>CC1C(=CC2=C(C=CC=C12)C)C(=O)Cl
O[C:10]([C:9]1=[CH:8][c:7]2[c:2]([CH3:1])[cH:3][cH:4][cH:5][c:6]2[CH:13]1[CH3:14])=[O:11].O=S(Cl)[Cl:12]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[c:7]1[CH:8]=[C:9]([C:10](=[O:11])[Cl:12])[CH:13]2[CH3:14]
Cc1cccc2c1C=C(C(=O)O)C2C.O=S(Cl)Cl
Cc1cccc2c1C=C(C(=O)Cl)C2C
null
null
null
Functional Group Interconversion
Alcohol to chloride_SOCl2
c301c14a9dcd0670d52e8b77396cbe7fd8edeedd757bc43f4162ade1fc52fc93
787f545db5dc0b29dde55b5fbed7db8625b8055f49327f97ed4d83cc47c3af1d
C1=Cc2ccccc2C1
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](=[C:5]-[c:6])-[C:7]>>[C:7]-[C:4](-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3])=[C:5]-[c:6]
100
[{"value": 100.0, "product": "CC1C(=CC2=C(C=CC=C12)C)C(=O)Cl", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
1,4-Dimethyl-indene-2-carboxylic acid is converted to its acid chloride by treatment with thionyl chloride. Yield 100%. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Acyl halide
null
null
C1=Cc2ccccc2C1
HCl
null
null
null
Cc1cccc2c1C=C(C(=O)O)C2C.O=S(Cl)Cl>>Cc1cccc2c1C=C(C(=O)Cl)C2C
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-28e41baf097a49e6ac6270dddced12dd
Cc1cccc2c1C=C(C(=O)O)C2C>>Cc1cccc2c1C[C@H](C(=O)O)[C@@H]2C
CC1C(=CC2=C(C=CC=C12)C)C(=O)O>>C[C@H]1[C@H](CC2=C(C=CC=C12)C)C(=O)O
[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[c:7]1[CH:8]=[C:9]([C:10](=[O:11])[OH:12])[CH:13]2[CH3:14]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[c:7]1[CH2:8][C@H:9]([C:10](=[O:11])[OH:12])[C@@H:13]2[CH3:14]
Cc1cccc2c1C=C(C(=O)O)C2C
Cc1cccc2c1C[C@H](C(=O)O)[C@@H]2C
null
[Pd]
C(C)O.O
Reduction
Hydrogenation (double to single)
e5689a02f639e60b4fe706a412d3f57570263b52462fa8286db9a999fcbf7a7c
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1ccc2c(c1)CCC2
[C;D1;H3:1]-[CH;D3;+0:2]1-[C;H0;D3;+0:3](-[C:4](=[O;D1;H0:5])-[O;D1;H1:6])=[CH;D2;+0:7]-[c:8](:[c:9]):[c:10]-1:[c:11]>>[C;D1;H3:1]-[C@H;D3;+0:2]1-[C@@H;D3;+0:3](-[C:4](=[O;D1;H0:5])-[O;D1;H1:6])-[CH2;D2;+0:7]-[c:8](:[c:9]):[c:10]-1:[c:11]
null
[]
null
null
null
null
1,4-Dimethyl-indene-2-carboxylic acid (35.5 g) is hydrogenated in ethanol-water (700 ml-70 ml) over 10% palladium on carbon at ambient temperature. After filtration ethanol is evaporated. Water is added and the precipitated cis-2,3-dihydro-1,4-dimethyl-1H-indene-2-carboxylic acid is filrated. Yield 33.3 g, 93% M.p. 132...
10.6084/m9.figshare.5104873.v1
null
null
null
C1=Cc2ccccc2C1
c1ccc2c(c1)CCC2
c1ccc2c(c1)CCC2
null
[Pd].C(C)O.O
null
null
Cc1cccc2c1C=C(C(=O)O)C2C>[Pd].C(C)O.O>Cc1cccc2c1C[C@H](C(=O)O)[C@@H]2C
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-a6468257cde240678537a92584eedbfd
Cc1cccc2c1C[C@H](C(=O)O)[C@@H]2C.O=S(Cl)Cl>>Cc1cccc2c1C[C@H](C(=O)Cl)[C@@H]2C
C[C@H]1[C@H](CC2=C(C=CC=C12)C)C(=O)O.S(=O)(Cl)Cl>>C[C@H]1[C@H](CC2=C(C=CC=C12)C)C(=O)Cl
O[C:10]([C@H:9]1[CH2:8][c:7]2[c:2]([CH3:1])[cH:3][cH:4][cH:5][c:6]2[C@H:13]1[CH3:14])=[O:11].O=S(Cl)[Cl:12]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[c:7]1[CH2:8][C@H:9]([C:10](=[O:11])[Cl:12])[C@@H:13]2[CH3:14]
Cc1cccc2c1C[C@H](C(=O)O)[C@@H]2C.O=S(Cl)Cl
Cc1cccc2c1C[C@H](C(=O)Cl)[C@@H]2C
null
null
null
Functional Group Interconversion
Alcohol to chloride_SOCl2
c301c14a9dcd0670d52e8b77396cbe7fd8edeedd757bc43f4162ade1fc52fc93
787f545db5dc0b29dde55b5fbed7db8625b8055f49327f97ed4d83cc47c3af1d
c1ccc2c(c1)CCC2
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](-[C:5])-[C:6]>>[C:5]-[C:4](-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3])-[C:6]
92
[{"value": 92.0, "product": "C[C@H]1[C@H](CC2=C(C=CC=C12)C)C(=O)Cl", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
cis-2,3-Dihydro-1,4-dimethyl-1H-indene-2-carboxylic acid is converted to its acid chloride by treatment with thionyl chloride. Yield 92%. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Acyl halide
null
null
c1ccc2c(c1)CCC2
HCl
null
null
null
Cc1cccc2c1C[C@H](C(=O)O)[C@@H]2C.O=S(Cl)Cl>>Cc1cccc2c1C[C@H](C(=O)Cl)[C@@H]2C
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-1b094d5a56494e2da452893b6b974dbc
CC1(C(=O)O)Cc2ccccc2C1.O=S(Cl)Cl>>CC1(C(=O)Cl)Cc2ccccc2C1
CC1(CC2=CC=CC=C2C1)C(=O)O.S(=O)(Cl)Cl>>CC1(CC2=CC=CC=C2C1)C(=O)Cl
O[C:3]([C:2]1([CH3:1])[CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[CH2:13]1)=[O:4].O=S(Cl)[Cl:5]>>[CH3:1][C:2]1([C:3](=[O:4])[Cl:5])[CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[CH2:13]1
CC1(C(=O)O)Cc2ccccc2C1.O=S(Cl)Cl
CC1(C(=O)Cl)Cc2ccccc2C1
null
null
null
Functional Group Interconversion
Alcohol to chloride_SOCl2
c301c14a9dcd0670d52e8b77396cbe7fd8edeedd757bc43f4162ade1fc52fc93
787f545db5dc0b29dde55b5fbed7db8625b8055f49327f97ed4d83cc47c3af1d
c1ccc2c(c1)CCC2
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](-[C;D1;H3:5])(-[C:6])-[C:7]>>[C:6]-[C:4](-[C;D1;H3:5])(-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3])-[C:7]
null
[]
null
null
null
null
A stirred mixture of 2,3-dihydro-2-methyl-1H-indene-2-carboxylic acid (6.70 g) and thionyl chloride (70 ml) is heated under reflux for 14 hr. The ecess of thionyl chloride is removed and the acid chloride is distilled. Yield 5.35 g, 72%, bp. 93°-98° C./3 mmHg. Conditions: See reaction.notes.procedure_details. Workup: i...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Acyl halide
null
null
c1ccc2c(c1)CCC2
HCl
null
null
null
CC1(C(=O)O)Cc2ccccc2C1.O=S(Cl)Cl>>CC1(C(=O)Cl)Cc2ccccc2C1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-85a2fa7645354306a0bcb4aae40fe67f
BrBr.CC(=O)C1(C)Cc2ccccc2C1>>CC1(C(=O)CBr)Cc2ccccc2C1
CC1(CC2=CC=CC=C2C1)C(C)=O.BrBr>>BrCC(=O)C1(CC2=CC=CC=C2C1)C
Br[Br:6].[CH3:1][C:2]1([C:3](=[O:4])[CH3:5])[CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[CH2:14]1>>[CH3:1][C:2]1([C:3](=[O:4])[CH2:5][Br:6])[CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[CH2:14]1
BrBr.CC(=O)C1(C)Cc2ccccc2C1
CC1(C(=O)CBr)Cc2ccccc2C1
null
null
C(Cl)Cl
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccc2c(c1)CCC2
Br-[Br;H0;D1;+0:1].[C:2]-[C:3](-[CH3;D1;+0:4])=[O;D1;H0:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:4]-[C:3](-[C:2])=[O;D1;H0:5]
null
[]
null
null
null
null
1-(2,3-Dihydro-2-methyl-1H-inden-2-yl)ethanone (3.69 g) in methylene chloride (40 ml) is stirred and cooled at 10° C. during the dropwise addition of bromine (2.82 g)/methylene chloride (10 ml). Work-up of the resultant solution gives 2-bromo-1-(2,3-dihydro-2-methyl-1H-inden-2-yl)ethanone. Conditions: See reaction.note...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccc2c(c1)CCC2
HBr
C(Cl)Cl
null
null
BrBr.CC(=O)C1(C)Cc2ccccc2C1>C(Cl)Cl>CC1(C(=O)CBr)Cc2ccccc2C1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-e661ba1483df42c9a16946f9259de1b6
BrC1Cc2ccccc2C1.CCOC(OCC)C(=O)NN1CCCCC1>>CCOC(C=O)(OCC)C1Cc2ccccc2C1
N1(CCCCC1)NC(C(OCC)OCC)=O.[Mg].[Mg].S(O)(O)(=O)=O.BrC1CC2=CC=CC=C2C1>>C(C)OC(C=O)(C1CC2=CC=CC=C2C1)OCC
Br[CH:10]1[CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[CH2:18]1.C1CCN(N[C:5]([CH:4]([O:3][CH2:2][CH3:1])[O:7][CH2:8][CH3:9])=[O:6])CC1>>[CH3:1][CH2:2][O:3][C:4]([CH:5]=[O:6])([O:7][CH2:8][CH3:9])[CH:10]1[CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[CH2:18]1
BrC1Cc2ccccc2C1.CCOC(OCC)C(=O)NN1CCCCC1
CCOC(C=O)(OCC)C1Cc2ccccc2C1
null
null
C(C)OCC
C-C Coupling
OtherReaction
33ad6fc0f5c61ff6e607266e8535db15f86926f49630c404b02f60eb84280f5c
96d7be43d301ef432c38e0dcab15db38e6b746a28e4247b22cb5e21a9e836c25
c1ccc2c(c1)CCC2
Br-[CH;D3;+0:1]1-[C:2]-[c:3]:[c:4]-[C:5]-1.[C:6]-[#8:7]-[CH;D3;+0:8](-[#8:9]-[C:10])-[C;H0;D3;+0:11](=[O;D1;H0:12])-N-N1-C-C-C-C-C-1>>[C:6]-[#8:7]-[C;H0;D4;+0:8](-[#8:9]-[C:10])(-[CH;D2;+0:11]=[O;D1;H0:12])-[CH;D3;+0:1]1-[C:2]-[c:3]:[c:4]-[C:5]-1
null
[]
null
null
2
HOUR
0.73 g of magnesium turnings are covered with 90 ml of dry diethylether. To that mixture is then added 6 g of 2-bromoindane in 20 ml of dry diethylether at such a rate that a gentle boiling is maintained. When the magnesium turnings have reacted the solution containing the Grignard reagent is cooled to room temperature...
10.6084/m9.figshare.5104873.v1
null
Acylhydrazine.Secondary halide.Ether.Ether
Aldehyde.Ether.Ether
c1ccc2c(c1)CCC2.C1CCNCC1
c1ccc2c(c1)CCC2
c1ccc2c(c1)CCC2
HBr
C(C)OCC
null
2
BrC1Cc2ccccc2C1.CCOC(OCC)C(=O)NN1CCCCC1>C(C)OCC>CCOC(C=O)(OCC)C1Cc2ccccc2C1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-107362592a79411db3a3bb2ea321f094
CCC1(C(=O)O)CCc2ccccc2C1.O=S(Cl)Cl>>CCC1(C(=O)Cl)CCc2ccccc2C1
C(C)C1(CC2=CC=CC=C2CC1)C(=O)O.S(=O)(Cl)Cl>>C(C)C1(CC2=CC=CC=C2CC1)C(=O)Cl
O[C:4]([C:3]1([CH2:2][CH3:1])[CH2:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]2[CH2:15]1)=[O:5].O=S(Cl)[Cl:6]>>[CH3:1][CH2:2][C:3]1([C:4](=[O:5])[Cl:6])[CH2:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]2[CH2:15]1
CCC1(C(=O)O)CCc2ccccc2C1.O=S(Cl)Cl
CCC1(C(=O)Cl)CCc2ccccc2C1
null
null
null
Functional Group Interconversion
Alcohol to chloride_SOCl2
c301c14a9dcd0670d52e8b77396cbe7fd8edeedd757bc43f4162ade1fc52fc93
787f545db5dc0b29dde55b5fbed7db8625b8055f49327f97ed4d83cc47c3af1d
c1ccc2c(c1)CCCC2
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](-[C:5])(-[C:6])-[C:7]>>[C:6]-[C:4](-[C:5])(-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3])-[C:7]
null
[]
null
null
5
DAY
A mixture of 2-ethyl-1,2,3,4-tetrahydro-2-naphthoic acid (22,0 g) and thionyl chloride is boiled for 5 days. The acid chloride is distilled. B.p. 110°-115° C./0.2 mmHg. Yield 21.6 g, 90%. Conditions: See reaction.notes.procedure_details. Workup: The acid chloride is distilled
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Acyl halide
null
null
c1ccc2c(c1)CCCC2
HCl
null
null
120
CCC1(C(=O)O)CCc2ccccc2C1.O=S(Cl)Cl>>CCC1(C(=O)Cl)CCc2ccccc2C1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-b78c327e1a3641088d5f502f89c88f70
CO.C[C@@H]1c2ccccc2C[C@@H]1C(=O)O>>COC(=O)[C@H]1Cc2ccccc2[C@H]1C
S(O)(O)(=O)=O.C[C@H]1[C@H](CC2=CC=CC=C12)C(=O)O.CO>>COC(=O)[C@@H]1[C@@H](C2=CC=CC=C2C1)C
[CH3:1][OH:2].O[C:3](=[O:4])[C@H:5]1[CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[C@H:13]1[CH3:14]>>[CH3:1][O:2][C:3](=[O:4])[C@H:5]1[CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[C@H:13]1[CH3:14]
CO.C[C@@H]1c2ccccc2C[C@@H]1C(=O)O
COC(=O)[C@H]1Cc2ccccc2[C@H]1C
null
null
null
Protection
Esterification of Carboxylic Acids
9cecdbd189c6f9c3648521d17154d013842a5498de4e76e65efb1d842973340b
af0b8064f2e82ebe66c4c29d2391785ac1b993104265ccdc4d67ca79e36fa3c8
c1ccc2c(c1)CCC2
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5].[C;D1;H3:6]-[OH;D1;+0:7]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[O;H0;D2;+0:7]-[C;D1;H3:6])-[C:5]
91
[{"value": 91.0, "product": "COC(=O)[C@@H]1[C@@H](C2=CC=CC=C2C1)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
cis-2,3-Dihydro-1-methyl-1H-indene-2-carboxylic acid methyl ester is prepared from cis-2,3-dihydro-1-methyl-1H-indene-2-carboxylic acid (see Example 4) by the standard methods using methanol and concentrated sulphuric acid. Yield 91%. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Methanol
Ester
null
null
c1ccc2c(c1)CCC2
HO-
null
null
null
CO.C[C@@H]1c2ccccc2C[C@@H]1C(=O)O>>COC(=O)[C@H]1Cc2ccccc2[C@H]1C
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-9d4ebd8e481047809b51612b904aa6b8
BrBr.CCC1(C(C)=O)Cc2ccccc2C1C>>CCC1(C(=O)CBr)Cc2ccccc2C1C
C(C)C1(C(C2=CC=CC=C2C1)C)C(C)=O.BrBr>>BrCC(=O)C1(C(C2=CC=CC=C2C1)C)CC
Br[Br:7].[CH3:1][CH2:2][C:3]1([C:4](=[O:5])[CH3:6])[CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]2[CH:15]1[CH3:16]>>[CH3:1][CH2:2][C:3]1([C:4](=[O:5])[CH2:6][Br:7])[CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]2[CH:15]1[CH3:16]
BrBr.CCC1(C(C)=O)Cc2ccccc2C1C
CCC1(C(=O)CBr)Cc2ccccc2C1C
null
null
C(Cl)Cl
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccc2c(c1)CCC2
Br-[Br;H0;D1;+0:1].[C:2]-[C:3](-[CH3;D1;+0:4])=[O;D1;H0:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:4]-[C:3](-[C:2])=[O;D1;H0:5]
65
[{"value": 65.0, "product": "BrCC(=O)C1(C(C2=CC=CC=C2C1)C)CC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Bromo-1-(2,3-dihydro-2-ethyl-1-methyl-1H-inden-2-yl)ethanone is prepared from 1-(2,3-dihydro-2-ethyl-1-methyl-1H-inden-2-yl)ethanone (21.6 g) by treatment with bromine (17.6 g) in methylene chloride (300 ml). Yield 65%. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccc2c(c1)CCC2
HBr
C(Cl)Cl
null
null
BrBr.CCC1(C(C)=O)Cc2ccccc2C1C>C(Cl)Cl>CCC1(C(=O)CBr)Cc2ccccc2C1C
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-0c50a0db96974d4e998373adf507d6e8
CC(=O)OC(C)=O.Nc1ccc(S(=O)(=O)O)c2ccccc12>>CC(=O)Nc1ccc(S(=O)(=O)O)c2ccccc12
NC1=CC=C(C2=CC=CC=C12)S(=O)(=O)O.N1=CC=CC=C1.C(C)(=O)OC(C)=O>>C(C)(=O)NC1=CC=C(C2=CC=CC=C12)S(=O)(=O)O.N1=CC=CC=C1
CC(=O)O[C:2]([CH3:1])=[O:3].[NH2:4][c:5]1[cH:6][cH:7][c:8]([S:9](=[O:10])(=[O:11])[OH:12])[c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]([S:9](=[O:10])(=[O:11])[OH:12])[c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12
CC(=O)OC(C)=O.Nc1ccc(S(=O)(=O)O)c2ccccc12
CC(=O)Nc1ccc(S(=O)(=O)O)c2ccccc12
null
null
C(C)O
Acylation
Aminolysis of esters
87d35e51b477fc9a658a6f307eb56d84c8879182772c9dd3a42ec0d584fd2684
627cbc0550c9f51ad0105d9fcf46677e8c93bed87ee95bfe69292a82550c95b7
c1ccc2ccccc2c1
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[NH;D2;+0:4]-[c:5](:[c:6]):[c:7]
59.4
[{"value": 59.4, "product": "C(C)(=O)NC1=CC=C(C2=CC=CC=C12)S(=O)(=O)O.N1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
12 g (0.05 mole) of 1-amino-4-naphthalenesulphonic acid, 7.2 ml of pyridine and 15 ml of acetic anhydride are placed in a flask provided with a stirrer and heater. The mixture is heated until the solution is clear, at which point 10 ml of absolute ethanol is added and the mixture is allowed to cool, first to ambient te...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Primary amine
Secondary amide
null
null
c1ccc2ccccc2c1
HO-
C(C)O
null
3
CC(=O)OC(C)=O.Nc1ccc(S(=O)(=O)O)c2ccccc12>C(C)O>CC(=O)Nc1ccc(S(=O)(=O)O)c2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-633630798e4d4a5bb72b060b5562efd4
CCN.CSC(=NC#N)NC1CCCc2ccccc21>>CCNC(=NC#N)NC1CCCc2ccccc21
C(#N)N=C(NC1CCCC2=CC=CC=C12)SC.C(C)N>>C(#N)N=C(NCC)NC1CCCC2=CC=CC=C12
[CH3:1][CH2:2][NH2:3].CS[C:4](=[N:5][C:6]#[N:7])[NH:8][CH:9]1[CH2:10][CH2:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]21>>[CH3:1][CH2:2][NH:3][C:4](=[N:5][C:6]#[N:7])[NH:8][CH:9]1[CH2:10][CH2:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]21
CCN.CSC(=NC#N)NC1CCCc2ccccc21
CCNC(=NC#N)NC1CCCc2ccccc21
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
2ebe33ae3b7bb48bd968f9b830d6d3b488b85670dea18c3fe37a1f418e787d67
88e0224d19b2dce8f9987d52554afb32090d36ff7ee19e89dc5bf66d30974ec4
c1ccc2c(c1)CCCC2
C-S-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[#7:5]-[C:6].[C;D1;H3:7]-[C:8]-[NH2;D1;+0:9]>>[C:6]-[#7:5]-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[NH;D2;+0:9]-[C:8]-[C;D1;H3:7]
null
[]
null
null
20
HOUR
A solution of 6.13 g of N'-cyano-N-(1,2,3,4-tetrahydro-1-naphthyl)-S-methylisothiourea and 10 ml of 70% aqueous ethylamine in 90 ml of ethanol was heated at reflux with stirring for 20 hours. The reaction mixture was cooled in a refrigerator to give 2.44 g of N"-cyano-N-ethyl-N'-(1,2,3,4-tetrahydro-1-naphthyl)guanidine...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Monosulfide
Secondary amine
null
null
c1ccc2c(c1)CCCC2
Other
C(C)O
null
20
CCN.CSC(=NC#N)NC1CCCc2ccccc21>C(C)O>CCNC(=NC#N)NC1CCCc2ccccc21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-4b4b32ae47a846a4bd3b2b48f365e3b5
CC(C)N.CSC(=NC#N)NC1CCCc2ccccc21>>CC(C)NC(=NC#N)NC1CCCc2ccccc21
C(#N)N=C(NC1CCCC2=CC=CC=C12)SC.C(C)(C)N>>C(#N)N=C(NC(C)C)NC1CCCC2=CC=CC=C12
[CH3:1][CH:2]([CH3:3])[NH2:4].CS[C:5](=[N:6][C:7]#[N:8])[NH:9][CH:10]1[CH2:11][CH2:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]21>>[CH3:1][CH:2]([CH3:3])[NH:4][C:5](=[N:6][C:7]#[N:8])[NH:9][CH:10]1[CH2:11][CH2:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]21
CC(C)N.CSC(=NC#N)NC1CCCc2ccccc21
CC(C)NC(=NC#N)NC1CCCc2ccccc21
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
2ebe33ae3b7bb48bd968f9b830d6d3b488b85670dea18c3fe37a1f418e787d67
88e0224d19b2dce8f9987d52554afb32090d36ff7ee19e89dc5bf66d30974ec4
c1ccc2c(c1)CCCC2
C-S-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[#7:5]-[C:6].[C;D1;H3:7]-[C:8](-[C;D1;H3:9])-[NH2;D1;+0:10]>>[C:6]-[#7:5]-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[NH;D2;+0:10]-[C:8](-[C;D1;H3:7])-[C;D1;H3:9]
null
[]
null
null
154
HOUR
A solution of 30.0 g of N'-cyano-N-(1,2,3,4-tetrahydro-1-napthyl)-S-methylisothiourea and 40 ml of isopropylamine in 300 ml of acetonitrile was heated at reflux with stirring for 154 hours. The solvent and excess isopropylamine were removed by evaporation in vacuo, leaving the crude product as a tacky, white solid. Cry...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Monosulfide
Secondary amine
null
null
c1ccc2c(c1)CCCC2
Other
C(C)#N
null
154
CC(C)N.CSC(=NC#N)NC1CCCc2ccccc21>C(C)#N>CC(C)NC(=NC#N)NC1CCCc2ccccc21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-304c38d018044bb286d8a97c383e9f1c
CCCN.CSC(=NC#N)NC1CCCc2ccccc21>>CCCNC(=NC#N)NC1CCCc2ccccc21
C(#N)N=C(NC1CCCC2=CC=CC=C12)SC.C(CC)N>>C(#N)N=C(NCCC)NC1CCCC2=CC=CC=C12
[CH3:1][CH2:2][CH2:3][NH2:4].CS[C:5](=[N:6][C:7]#[N:8])[NH:9][CH:10]1[CH2:11][CH2:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]21>>[CH3:1][CH2:2][CH2:3][NH:4][C:5](=[N:6][C:7]#[N:8])[NH:9][CH:10]1[CH2:11][CH2:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]21
CCCN.CSC(=NC#N)NC1CCCc2ccccc21
CCCNC(=NC#N)NC1CCCc2ccccc21
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
2ebe33ae3b7bb48bd968f9b830d6d3b488b85670dea18c3fe37a1f418e787d67
88e0224d19b2dce8f9987d52554afb32090d36ff7ee19e89dc5bf66d30974ec4
c1ccc2c(c1)CCCC2
C-S-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[#7:5]-[C:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:6]-[#7:5]-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[NH;D2;+0:9]-[C:8]-[C:7]
null
[]
null
null
20
HOUR
A solution of 12.3 g of N'-cyano-N-(1,2,3,4-tetrahydro-1-napthyl)-S-methylisothiourea and 16 ml of n-propylamine in 100 ml of acetonitrile was heated at reflux with stirring for 20 hours. The reaction mixture was then allowed to stand in a refrigerator to give 8.63 g of N"-cyano-N-n-propyl-N'-(1,2,3,4-tetrahydro-1-naph...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Monosulfide
Secondary amine
null
null
c1ccc2c(c1)CCCC2
Other
C(C)#N
null
20
CCCN.CSC(=NC#N)NC1CCCc2ccccc21>C(C)#N>CCCNC(=NC#N)NC1CCCc2ccccc21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-7f6895ba5ca84377a6aeef1d151e9b4b
CN.CSC(=NC#N)NC1CCCc2ccccc21>>CNC(=NC#N)NC1CCCc2ccccc21
C(#N)N=C(NC1CCCC2=CC=CC=C12)SC.CN>>C(#N)N=C(NC)NC1CCCC2=CC=CC=C12
[CH3:1][NH2:2].CS[C:3](=[N:4][C:5]#[N:6])[NH:7][CH:8]1[CH2:9][CH2:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]21>>[CH3:1][NH:2][C:3](=[N:4][C:5]#[N:6])[NH:7][CH:8]1[CH2:9][CH2:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]21
CN.CSC(=NC#N)NC1CCCc2ccccc21
CNC(=NC#N)NC1CCCc2ccccc21
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
2ebe33ae3b7bb48bd968f9b830d6d3b488b85670dea18c3fe37a1f418e787d67
88e0224d19b2dce8f9987d52554afb32090d36ff7ee19e89dc5bf66d30974ec4
c1ccc2c(c1)CCCC2
C-S-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[#7:5]-[C:6].[C;D1;H3:7]-[NH2;D1;+0:8]>>[C:6]-[#7:5]-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[NH;D2;+0:8]-[C;D1;H3:7]
null
[]
null
null
22
HOUR
A solution of 12.3 g of N'-cyano-N-(1,2,3,4-tetrahydro-1-naphthyl)-S-methylisothiourea and 20 ml of 33% ethanolic methylamine in 200 ml of ethanol was heated at reflux with stirring for 22 hours. The solvent was then removed by evaporation in vacuo, leaving the crude product as a glassy, amorphous solid. Crystallizatio...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Monosulfide
Secondary amine
null
null
c1ccc2c(c1)CCCC2
Other
C(C)O
null
22
CN.CSC(=NC#N)NC1CCCc2ccccc21>C(C)O>CNC(=NC#N)NC1CCCc2ccccc21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-b9959cbcabf24a84aa148b8ecad25cdc
C=CCN.CSC(=NC#N)NC1CCCc2ccccc21>>C=CCNC(=NC#N)NC1CCCc2ccccc21
C(#N)N=C(NC1CCCC2=CC=CC=C12)SC.C(C=C)N>>C(C=C)NC(=NC#N)NC1CCCC2=CC=CC=C12
[CH2:1]=[CH:2][CH2:3][NH2:4].CS[C:5](=[N:6][C:7]#[N:8])[NH:9][CH:10]1[CH2:11][CH2:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]21>>[CH2:1]=[CH:2][CH2:3][NH:4][C:5](=[N:6][C:7]#[N:8])[NH:9][CH:10]1[CH2:11][CH2:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]21
C=CCN.CSC(=NC#N)NC1CCCc2ccccc21
C=CCNC(=NC#N)NC1CCCc2ccccc21
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
2ebe33ae3b7bb48bd968f9b830d6d3b488b85670dea18c3fe37a1f418e787d67
88e0224d19b2dce8f9987d52554afb32090d36ff7ee19e89dc5bf66d30974ec4
c1ccc2c(c1)CCCC2
C-S-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[#7:5]-[C:6].[C;D1;H2:7]=[C:8]-[C:9]-[NH2;D1;+0:10]>>[C:6]-[#7:5]-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[NH;D2;+0:10]-[C:9]-[C:8]=[C;D1;H2:7]
null
[]
null
null
null
null
A solution of 24.5 g of N'-cyano-N-(1,2,3,4-tetrahydro-1-naphthyl)-S-methylisothiourea and 38 ml of allylamine in 400 ml of ethanol was heated at reflux for 87 hours. The solvent was removed from the reaction mixture by evaporation in vacuo, leaving a pale yellow semisolid which was crystallized from isopropyl acetate ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Monosulfide
Secondary amine
null
null
c1ccc2c(c1)CCCC2
Other
C(C)O
null
null
C=CCN.CSC(=NC#N)NC1CCCc2ccccc21>C(C)O>C=CCNC(=NC#N)NC1CCCc2ccccc21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-2a25a670f29446a8bcfed9c8a1b1ea10
CC(C)CN.O=[N+]([O-])c1cnc2ccccc2c1Cl>>CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12
ClC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-].C(C(C)C)N>>C(C(C)C)NC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]
[CH3:1][CH:2]([CH3:3])[CH2:4][NH2:5].Cl[c:6]1[c:7]([N+:8](=[O:9])[O-:10])[cH:11][n:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12>>[CH3:1][CH:2]([CH3:3])[CH2:4][NH:5][c:6]1[c:7]([N+:8](=[O:9])[O-:10])[cH:11][n:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12
CC(C)CN.O=[N+]([O-])c1cnc2ccccc2c1Cl
CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2ncccc2c1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
null
[]
null
null
null
null
To a stirred solution of 50.Og (0.24 mole) of 4-chloro-3-nitroquinoline in 300 ml of tetrahydrofuran was added, in small portions, 52.7g (0.72 mole) of isobutylamine. The mixture was heated at its reflux temperature for one hour, and was then evaporated in vacuo. Water was added to the residue and the solid was separat...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
O1CCCC1
null
null
CC(C)CN.O=[N+]([O-])c1cnc2ccccc2c1Cl>O1CCCC1>CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-701fcea6be6145faa217161bfc2ee4fd
CN.O=[N+]([O-])c1cnc2ccccc2c1Cl>>CNc1c([N+](=O)[O-])cnc2ccccc12
CN.ClC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]>>CNC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]
[CH3:1][NH2:2].Cl[c:3]1[c:4]([N+:5](=[O:6])[O-:7])[cH:8][n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]12>>[CH3:1][NH:2][c:3]1[c:4]([N+:5](=[O:6])[O-:7])[cH:8][n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]12
CN.O=[N+]([O-])c1cnc2ccccc2c1Cl
CNc1c([N+](=O)[O-])cnc2ccccc12
null
null
O
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2ncccc2c1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C;D1;H3:10]-[NH2;D1;+0:11]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:11]-[C;D1;H3:10]
null
[]
null
null
null
null
To a stirred solution of 40% aqueous methylamine was added, in small portions, 30.Og (0.144 mole) of 4-chloro-3-nitroquinoline. The reaction mixture was heated at its reflux temperature for about 0.75 hour. After cooling, the mixture was poured into 300 ml of water. The solid was separated by filtration, and was then s...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
O
null
null
CN.O=[N+]([O-])c1cnc2ccccc2c1Cl>O>CNc1c([N+](=O)[O-])cnc2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-140b435f511a4d6abe847ad623279805
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl>>CC(C)Cn1cnc2c(Cl)nc3ccccc3c21
C(C(C)C)N1C=NC=2C=[N+](C=3C=CC=CC3C21)[O-].P(=O)(Cl)(Cl)Cl>>ClC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)C
[O-][n+:11]1[cH:9][c:8]2[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:18]2[c:17]2[c:12]1[cH:13][cH:14][cH:15][cH:16]2.O=P(Cl)(Cl)[Cl:10]>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([Cl:10])[n:11][c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[c:18]12
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21
null
null
null
Miscellaneous
OtherReaction
c5cfc3e69c2d1a66a8560034fe025f449600689a18546e68a564dc97632a28be
a48150e9dff88baab32dd83daf5ab089c597626e3c583c33a5868d8e1353c1ea
c1ccc2c(c1)ncc1nc[nH]c12
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[cH;D2;+0:7]:[n+;H0;D3:8](-[O-]):[c:9](:[c:10]):[c:11]:[c:12]:1:2>>[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[c:12]:1:[c:11]:[c:9](:[c:10]):[n;H0;D2;+0:8]:[c;H0;D3;+0:7]:2-[Cl;H0;D1;+0:1]
null
[]
null
null
null
null
A mixture of 9.95 g (0.0412 mole) of 1-isobutyl-1H-imidazo [4,5-c]quinolin-5-oxide (from Example 54) and 100 ml of phosphorus oxychloride was heated at its reflux temperature for 2.5 hours, and was then cooled and poured into ice with stirring. Basification (to pH 9-10) with 50% aqueous sodium hydroxide solution was fo...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2c(c1)[n+]cc1[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
HCl
null
null
null
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl>>CC(C)Cn1cnc2c(Cl)nc3ccccc3c21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-dbffeec5148f4326a5a271f967528eb5
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.[NH4+]>>CC(C)Cn1cnc2c(N)nc3ccccc3c21
ClC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)C.[OH-].[NH4+]>>C(C(C)C)N1C=NC=2C(=NC=3C=CC=CC3C21)N
Cl[c:9]1[c:8]2[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:18]2[c:17]2[c:12]([n:11]1)[cH:13][cH:14][cH:15][cH:16]2.[NH4+:10]>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[c:18]12
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.[NH4+]
CC(C)Cn1cnc2c(N)nc3ccccc3c21
null
null
null
Functional Group Interconversion
OtherReaction
5180f216097ba9fb57e932c038efbe236ac4870417fb61da74fdffde0a3037cf
560c85d40afb1a57d77cf3258abf3be5bba829f35224f8687bf9a1d4c1f94bd9
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c:5]2:[#7;a:6](-[C:7]):[c:8]:[#7;a:9]:[c:10]:2:1.[NH4+;D0:11]>>[C:7]-[#7;a:6]1:[c:8]:[#7;a:9]:[c:10]2:[c:5]:1:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:2-[NH2;D1;+0:11]
null
[]
150
CELSIUS
null
null
A mixture of 4.0 g (0.0154 mole) of 4-chloro-1-isobutyl-1H-imidazo [4,5-c]quinoline (from Example 77) and 25 cc of concentrated ammonium hydroxide was placed in a metal bomb and heated at 150° C. for about 16 hours. After cooling the solid was separated by filtration, washed with water and recrystallized from ethanol t...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
HCl
null
150
null
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.[NH4+]>>CC(C)Cn1cnc2c(N)nc3ccccc3c21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-e947c30edcac4d5f85af4d0febdc8b90
O=C(OCCn1cnc2cnc3ccccc3c21)c1ccccc1.OO>>O=C(OCCn1cnc2c[n+]([O-])c3ccccc3c21)c1ccccc1
C(C1=CC=CC=C1)(=O)OCCN1C=NC=2C=NC=3C=CC=CC3C21.OO>>C(C1=CC=CC=C1)(=O)OCCN1C=NC=2C=[N+](C=3C=CC=CC3C21)[O-]
[O:1]=[C:2]([O:3][CH2:4][CH2:5][n:6]1[cH:7][n:8][c:9]2[cH:10][n:11][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[c:19]12)[c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1.O[OH:12]>>[O:1]=[C:2]([O:3][CH2:4][CH2:5][n:6]1[cH:7][n:8][c:9]2[cH:10][n+:11]([O-:12])[c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[c:19]12)[c:20]1[cH:21][cH:22...
O=C(OCCn1cnc2cnc3ccccc3c21)c1ccccc1.OO
O=C(OCCn1cnc2c[n+]([O-])c3ccccc3c21)c1ccccc1
null
null
C(C)(=O)O
Functional Group Interconversion
OtherReaction
ad4e5886430ca643e61e33ce51381127eb6443ce8f7fd345eaa14b7a1d61bd3d
bf536f3bf8ed7b8faf08cf1c004ccd0a5e7fe59339402dd73ac837bb4a52f2ba
O=C(OCCn1cnc2c[nH+]c3ccccc3c21)c1ccccc1
O-[OH;D1;+0:1].[c:2]:[c:3]1:[c:4]:[c:5]2:[#7;a:6]:[c:7]:[#7;a:8]:[c:9]:2:[c:10]:[n;H0;D2;+0:11]:1>>[O-;H0;D1:1]-[n+;H0;D3:11]1:[c:10]:[c:9]2:[#7;a:8]:[c:7]:[#7;a:6]:[c:5]:2:[c:4]:[c:3]:1:[c:2]
null
[]
65
CELSIUS
null
null
A mixture of 67.5 g (0.213 mole) of 1-(2-benzoyloxyethyl)-1H-imidazo[4,5-c]quinoline (from Example 115), 36.3 g (0.32 mole) of 30% hydrogen peroxide and 450 ml of glacial acetic acid was heated at 65° C. for 2 days with stirring. The solution was evaporated in vacuo, and the residue was then added to water. The mixture...
10.6084/m9.figshare.5104873.v1
null
Peroxide
null
c1ccc2c(c1)ncc1nc[nH]c12
c1ccc2c(c1)[n+]cc1nc[nH]c12
c1ccc2c(c1)[n+]cc1nc[nH]c12.c1ccccc1
HO-
C(C)(=O)O
65
null
O=C(OCCn1cnc2cnc3ccccc3c21)c1ccccc1.OO>C(C)(=O)O>O=C(OCCn1cnc2c[n+]([O-])c3ccccc3c21)c1ccccc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-fd07e5c4703549e79fcc07e18a5b58b2
O=C(OCCn1cnc2c[n+]([O-])c3ccccc3c21)c1ccccc1.O=P(Cl)(Cl)Cl>>O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1
C(C1=CC=CC=C1)(=O)OCCN1C=NC=2C=[N+](C=3C=CC=CC3C21)[O-].P(=O)(Cl)(Cl)Cl>>C(C1=CC=CC=C1)(=O)OCCN1C=NC=2C(=NC=3C=CC=CC3C21)Cl
[O-][n+:12]1[cH:10][c:9]2[n:8][cH:7][n:6]([CH2:5][CH2:4][O:3][C:2](=[O:1])[c:20]3[cH:21][cH:22][cH:23][cH:24][cH:25]3)[c:19]2[c:18]2[c:13]1[cH:14][cH:15][cH:16][cH:17]2.O=P(Cl)(Cl)[Cl:11]>>[O:1]=[C:2]([O:3][CH2:4][CH2:5][n:6]1[cH:7][n:8][c:9]2[c:10]([Cl:11])[n:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[c:19]12)[c:20...
O=C(OCCn1cnc2c[n+]([O-])c3ccccc3c21)c1ccccc1.O=P(Cl)(Cl)Cl
O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1
null
null
null
Miscellaneous
OtherReaction
c5cfc3e69c2d1a66a8560034fe025f449600689a18546e68a564dc97632a28be
a48150e9dff88baab32dd83daf5ab089c597626e3c583c33a5868d8e1353c1ea
O=C(OCCn1cnc2cnc3ccccc3c21)c1ccccc1
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[cH;D2;+0:7]:[n+;H0;D3:8](-[O-]):[c:9](:[c:10]):[c:11]:[c:12]:1:2>>[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[c:12]:1:[c:11]:[c:9](:[c:10]):[n;H0;D2;+0:8]:[c;H0;D3;+0:7]:2-[Cl;H0;D1;+0:1]
null
[]
null
null
null
null
A mixture of 50g (0.15 mole) of 1-(2-benzoyloxyethyl)-1H-imidazo[4,5-c]quinolin-5-oxide (from Example 116) and 200 ml of phosphorus oxychloride was heated for two hours on a steam bath. The mixture was then partially evaporated in vacuo. The mixture was poured over ice, and the solution was neutralized with sodium hydr...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2c(c1)[n+]cc1[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12.c1ccccc1
HCl
null
null
null
O=C(OCCn1cnc2c[n+]([O-])c3ccccc3c21)c1ccccc1.O=P(Cl)(Cl)Cl>>O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-09412f2ea4984b9680a422f7d8c6366d
O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1>>OCCn1cnc2c(Cl)nc3ccccc3c21
C(C1=CC=CC=C1)(=O)OCCN1C=NC=2C(=NC=3C=CC=CC3C21)Cl.N>>ClC1=NC=2C=CC=CC2C2=C1N=CN2CCO
O=C(c1ccccc1)[O:1][CH2:2][CH2:3][n:4]1[cH:5][n:6][c:7]2[c:8]([Cl:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]12>>[OH:1][CH2:2][CH2:3][n:4]1[cH:5][n:6][c:7]2[c:8]([Cl:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]12
O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1
OCCn1cnc2c(Cl)nc3ccccc3c21
null
null
CO
Reduction
Hydrolysis or Hydrogenolysis of Carboxylic Esters or Thioesters
8df1b5c4ec88eb8f4e334a9ade2ac7fc0b3f460ea1450816d1758f28eee39662
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc2c(c1)ncc1nc[nH]c12
O=C(-[O;H0;D2;+0:1]-[C:2]-[C:3])-c1:c:c:c:c:c:1>>[C:3]-[C:2]-[OH;D1;+0:1]
null
[]
20
CELSIUS
3
DAY
A mixture of 25.3 g (0.072 mole) of 1-(2-benzoyloxyethyl)-4-chloro-1H-imidazo[4,5-c]quinoline (from Example 117) and 500 ml of 10% ammonia in methanol was stirred at about 20° C. for three days, and was then filtered and finally evaporated to low volume. The slurry was mixed with diethyl ether, and the solid was separa...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
c1ccccc1
null
c1nc2ccccc2c2[nH]cnc12
HO-
CO
20
72
O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1>CO>OCCn1cnc2c(Cl)nc3ccccc3c21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-d55cf3cb02ba41bab50cae8993ff9059
N.O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1>>Cl.Nc1nc2ccccc2c2c1ncn2CCO.O
C(C1=CC=CC=C1)(=O)OCCN1C=NC=2C(=NC=3C=CC=CC3C21)Cl.N>>O.Cl.OCCN1C=NC=2C(=NC=3C=CC=CC3C21)N
[NH3:2].c1ccc(C([O:18][CH2:17][CH2:16][n:15]2[c:11]3[c:10]4[c:5]([n:4][c:3]([Cl:1])[c:12]3[n:13][cH:14]2)[cH:6][cH:7][cH:8][cH:9]4)=[O:19])cc1>>[ClH:1].[NH2:2][c:3]1[n:4][c:5]2[cH:6][cH:7][cH:8][cH:9][c:10]2[c:11]2[c:12]1[n:13][cH:14][n:15]2[CH2:16][CH2:17][OH:18].[OH2:19]
N.O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1
Cl.Nc1nc2ccccc2c2c1ncn2CCO.O
null
null
Cl.CO
Heteroatom Alkylation and Arylation
OtherReaction
665ca0a8153959cf33011b69b672067ade7501393d2797d593ce4706bc4cf371
a0d2810f2e52e72d80187445295033f9d64ed41da4af71c56901ee260d67fe3b
c1ccc2c(c1)ncc1nc[nH]c12
[Cl;H0;D1;+0:1]-[c;H0;D3;+0:2]1:[#7;a:3]:[c:4]:[c:5]:[c:6]2:[#7;a:7](-[C:8]-[C:9]-[O;H0;D2;+0:10]-C(=[O;H0;D1;+0:11])-c3:c:c:c:c:c:3):[c:12]:[#7;a:13]:[c:14]:2:1.[NH3;D0;+0:15]>>[ClH;D0;+0:1].[NH2;D1;+0:15]-[c;H0;D3;+0:2]1:[#7;a:3]:[c:4]:[c:5]:[c:6]2:[#7;a:7](-[C:8]-[C:9]-[OH;D1;+0:10]):[c:12]:[#7;a:13]:[c:14]:2:1.[OH2...
null
[]
null
null
null
null
A mixture of 1.3 g (0.0037 mole) of 1-(2-benzoyloxyethyl)-4-chloro-1H-imidazo[4,5-c]quinoline (from Example 117) in 60 ml of methanol was saturated with about 10g of ammonia gas. The mixture was heated at 150° C. in a steel bomb for ten hours. The mixture was evaporated, and the residue was slurried in diethyl ether an...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ester
Primary alcohol.Primary amine
c1ccccc1.c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2nc[nH]c12
Other
Cl.CO
null
null
N.O=C(OCCn1cnc2c(Cl)nc3ccccc3c21)c1ccccc1>Cl.CO>Cl.Nc1nc2ccccc2c2c1ncn2CCO.O
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-b1be4dfd6da4477da37761d7f80d972c
O=C(Cl)c1ccccc1.OCC(O)Cn1cnc2cnc3ccccc3c21>>O=C(OCC(Cn1cnc2cnc3ccccc3c21)OC(=O)c1ccccc1)c1ccccc1
C(C1=CC=CC=C1)(=O)Cl.OC(CN1C=NC=2C=NC=3C=CC=CC3C21)CO>>C(C1=CC=CC=C1)(=O)OC(CN1C=NC=2C=NC=3C=CC=CC3C21)COC(C2=CC=CC=C2)=O
Cl[C:21](=[O:22])[c:23]1[cH:24][cH:25][cH:2][cH:27][cH:28]1.[OH:1][CH2:4][CH:5]([CH2:6][n:7]1[cH:8][n:9][c:10]2[cH:11][n:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[c:19]12)[OH:20]>>[O:1]=[C:2]([O:3][CH2:4][CH:5]([CH2:6][n:7]1[cH:8][n:9][c:10]2[cH:11][n:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[c:19]12)[O:20][C:2...
O=C(Cl)c1ccccc1.OCC(O)Cn1cnc2cnc3ccccc3c21
O=C(OCC(Cn1cnc2cnc3ccccc3c21)OC(=O)c1ccccc1)c1ccccc1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
6f2ba2a48e83b7d7a9ef833d61a803f978e1e5237808ad4cd37f7e0315e7bd3f
8eb99b12d7d9bf3bf89650dc1a9dd90efde0b77ac3da22794c3abe4e413897c2
O=C(OCC(Cn1cnc2cnc3ccccc3c21)OC(=O)c1ccccc1)c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[c:4]:[cH;D2;+0:5]:[cH;D2;+0:6]:[cH;D2;+0:7]:[c:8]:1.[C:9]-[C:10](-[OH;D1;+0:11])-[CH2;D2;+0:12]-[OH;D1;+0:13]>>[C:9]-[C:10](-[CH2;D2;+0:12]-[#8:14]-[C;H0;D3;+0:6](=[O;H0;D1;+0:13])-[c:15](:[c:16]):[c:17])-[O;H0;D2;+0:11]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[c:4]:[cH;D2;+0:5]:[c:1...
null
[]
null
null
null
null
Using the method of Example 115, benzoyl chloride was reacted with 1-(2,3-dihydroxypropyl)-1H-imidazo[4,5-c]-quinoline (from Example 51) to provide 1-(2,3-dibenzoyloxypropyl)-1H-imidazo[4,5-c]quinoline. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary alcohol.Secondary alcohol
Ester.Ester
c1ccccc1
c1ccccc1.c1ccccc1
c1ccc2c(c1)ncc1nc[nH]c12.c1ccccc1.c1ccccc1
null
null
null
null
O=C(Cl)c1ccccc1.OCC(O)Cn1cnc2cnc3ccccc3c21>>O=C(OCC(Cn1cnc2cnc3ccccc3c21)OC(=O)c1ccccc1)c1ccccc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-2c929c9ff91f46908204776551292b7d
CC(=O)OCC(Cn1cnc2c[n+]([O-])c3ccccc3c21)OC(C)=O>>[O-][n+]1cc2ncn(CC(O)CO)c2c2ccccc21
C(C)(=O)OC(CN1C=NC=2C=[N+](C=3C=CC=CC3C21)[O-])COC(C)=O>>OC(CN1C=NC=2C=[N+](C=3C=CC=CC3C21)[O-])CO
CC(=O)[O:10][CH:9]([CH2:8][n:7]1[cH:6][n:5][c:4]2[cH:3][n+:2]([O-:1])[c:19]3[c:14]([c:13]21)[cH:15][cH:16][cH:17][cH:18]3)[CH2:11][O:12]C(C)=O>>[O-:1][n+:2]1[cH:3][c:4]2[n:5][cH:6][n:7]([CH2:8][CH:9]([OH:10])[CH2:11][OH:12])[c:13]2[c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]12
CC(=O)OCC(Cn1cnc2c[n+]([O-])c3ccccc3c21)OC(C)=O
[O-][n+]1cc2ncn(CC(O)CO)c2c2ccccc21
null
C[O-].[Na+]
CO
Reduction
OtherReaction
729bb4ff95e38c3d11c4da55fe3e362074025f1fba900386729c8f4837142b9a
f7eaf12d8ca7f7f33975963ce6d5d64e20763721d3f59f4cd8cae1a62b7f8497
c1ccc2c(c1)[nH+]cc1nc[nH]c12
C-C(=O)-[O;H0;D2;+0:1]-[C:2](-[C:3])-[C:4]-[O;H0;D2;+0:5]-C(-C)=O>>[C:3]-[C:2](-[OH;D1;+0:1])-[C:4]-[OH;D1;+0:5]
null
[]
null
null
null
null
To a stirred solution of 4.0 g (0.0117 mole) of 1-(2,3-diacetoxypropyl)-1H-imidazo[4,5-c]quinolin-5-oxide (from Example 121, Part A) in 50 ml of methanol was added about 12 drops of 25% sodium methoxide solution. After one hour the product was collected by filtration, washed with methanol and recrystallized from ethano...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Primary alcohol.Secondary alcohol
null
null
c1ccc2c(c1)[n+]cc1[nH]cnc12
HO-
C[O-].[Na+].CO
null
null
CC(=O)OCC(Cn1cnc2c[n+]([O-])c3ccccc3c21)OC(C)=O>C[O-].[Na+].CO>[O-][n+]1cc2ncn(CC(O)CO)c2c2ccccc21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-cc6dcb2adf4e4ae7a8c81d53c0d50ebb
NCc1ccccc1.O=[N+]([O-])c1cnc2ccccc2c1Cl>>O=[N+]([O-])c1cnc2ccccc2c1NCc1ccccc1
C(C1=CC=CC=C1)N.ClC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]>>C(C1=CC=CC=C1)NC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]
[NH2:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1.Cl[c:13]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[c:13]1[NH:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1
NCc1ccccc1.O=[N+]([O-])c1cnc2ccccc2c1Cl
O=[N+]([O-])c1cnc2ccccc2c1NCc1ccccc1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(CNc2ccnc3ccccc23)cc1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[NH2;D1;+0:10]-[C:11]-[c:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:10]-[C:11]-[c:12]
null
[]
null
null
null
null
Using the method of Example 1, benzylamine and 4-chloro-3-nitroquinoline were reacted to provide 4-benzylamino-3-nitroquinoline. The structural assignment for the crude product (m.p. 178°-196° C.) was supported by infrared spectral analysis. Conditions: See reaction.notes.procedure_details. Workup: were reacted
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HCl
null
null
null
NCc1ccccc1.O=[N+]([O-])c1cnc2ccccc2c1Cl>>O=[N+]([O-])c1cnc2ccccc2c1NCc1ccccc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-f325f0d97a2d4a3d92dc24afc812f03e
Clc1nc2ccccc2c2c1ncn2Cc1ccccc1.N>>Nc1nc2ccccc2c2c1ncn2Cc1ccccc1
C(C1=CC=CC=C1)N1C=NC=2C(=NC=3C=CC=CC3C21)Cl.N>>C(C1=CC=CC=C1)N1C=NC=2C(=NC=3C=CC=CC3C21)N
Cl[c:2]1[n:3][c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[c:10]2[c:11]1[n:12][cH:13][n:14]2[CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1.[NH3:1]>>[NH2:1][c:2]1[n:3][c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[c:10]2[c:11]1[n:12][cH:13][n:14]2[CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1
Clc1nc2ccccc2c2c1ncn2Cc1ccccc1.N
Nc1nc2ccccc2c2c1ncn2Cc1ccccc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
a67570e0a22d637a1d2a31207671ab3b6e569ccedb0b9b67428b6008b9e1da93
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1ccc(Cn2cnc3cnc4ccccc4c32)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c:5]2:[#7;a:6](-[C:7]):[c:8]:[#7;a:9]:[c:10]:2:1.[NH3;D0;+0:11]>>[C:7]-[#7;a:6]1:[c:8]:[#7;a:9]:[c:10]2:[c:5]:1:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:2-[NH2;D1;+0:11]
null
[]
null
null
null
null
Using the method of Example 100, 1-benzyl-4-chloro-1H-imidazo[4,5-c]quinoline (from Example 80) was reacted with ammonia to provide white solid 1-benzyl-1H-imidazo[4,5-c]quinolin-4-amine after recrystallization from N,N-dimethylformamide, m.p. 257°-259° C. Analysis: Calculated for C17H14N4: % C, 74.4; % H, 5.1; % N, 20...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2nc[nH]c12.c1ccccc1
HCl
null
null
null
Clc1nc2ccccc2c2c1ncn2Cc1ccccc1.N>>Nc1nc2ccccc2c2c1ncn2Cc1ccccc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-70af8be2728549008f36c1cf9792bfa8
NCc1ccc(Cl)cc1.O=[N+]([O-])c1cnc2ccccc2c1Cl>>O=[N+]([O-])c1cnc2ccccc2c1NCc1ccc(Cl)cc1
ClC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-].ClC1=CC=C(CN)C=C1>>ClC1=CC=C(CNC2=C(C=NC3=CC=CC=C23)[N+](=O)[O-])C=C1
[NH2:14][CH2:15][c:16]1[cH:17][cH:18][c:19]([Cl:20])[cH:21][cH:22]1.Cl[c:13]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[c:13]1[NH:14][CH2:15][c:16]1[cH:17][cH:18][c:19]([Cl:20])[cH:21][cH:22]1
NCc1ccc(Cl)cc1.O=[N+]([O-])c1cnc2ccccc2c1Cl
O=[N+]([O-])c1cnc2ccccc2c1NCc1ccc(Cl)cc1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(CNc2ccnc3ccccc23)cc1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[NH2;D1;+0:10]-[C:11]-[c:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:10]-[C:11]-[c:12]
null
[]
null
null
null
null
Using the method of Example 1, 4-chloro-3-nitroquinoline was reacted with 4-chlorobenzylamine to provide yellow solid 4-(4-chlorobenzylamino)-3-nitroquinoline, the melting point of the crude product being 168°-173° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HCl
null
null
null
NCc1ccc(Cl)cc1.O=[N+]([O-])c1cnc2ccccc2c1Cl>>O=[N+]([O-])c1cnc2ccccc2c1NCc1ccc(Cl)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-8ef73e706205480ba66a62dbc024f1f3
NCCc1ccccc1.O=[N+]([O-])c1cnc2ccccc2c1Cl>>O=[N+]([O-])c1cnc2ccccc2c1NCCc1ccccc1
ClC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-].C1(=CC=CC=C1)CCN>>[N+](=O)([O-])C=1C=NC2=CC=CC=C2C1NCCC1=CC=CC=C1
[NH2:14][CH2:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1.Cl[c:13]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[c:13]1[NH:14][CH2:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1
NCCc1ccccc1.O=[N+]([O-])c1cnc2ccccc2c1Cl
O=[N+]([O-])c1cnc2ccccc2c1NCCc1ccccc1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(CCNc2ccnc3ccccc23)cc1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
null
[]
null
null
null
null
Using the method of Example 1, 4-chloro-3-nitroquinoline was reacted with 2-(phenyl)ethylamine to provide yellow solid 3-nitro-4-[2-(phenyl)ethylamino]quinoline, the melting point of the crude product being 174°-180° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HCl
null
null
null
NCCc1ccccc1.O=[N+]([O-])c1cnc2ccccc2c1Cl>>O=[N+]([O-])c1cnc2ccccc2c1NCCc1ccccc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-88618bfd351a40df87e724b2284ff983
Nc1cnc2ccccc2c1NCCc1ccccc1>>c1ccc(CCn2cnc3cnc4ccccc4c32)cc1
NC=1C=NC2=CC=CC=C2C1NCCC1=CC=CC=C1.C(OCC)(OCC)OCC>>C1(=CC=CC=C1)CCN1C=NC=2C=NC=3C=CC=CC3C21
[cH:1]1[cH:2][cH:3][c:4]([CH2:5][CH2:6][NH:7][c:19]2[c:10]([NH2:9])[cH:11][n:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]32)[cH:20][cH:21]1>>[cH:1]1[cH:2][cH:3][c:4]([CH2:5][CH2:6][n:7]2[cH:8][n:9][c:10]3[cH:11][n:12][c:13]4[cH:14][cH:15][cH:16][cH:17][c:18]4[c:19]23)[cH:20][cH:21]1
Nc1cnc2ccccc2c1NCCc1ccccc1
c1ccc(CCn2cnc3cnc4ccccc4c32)cc1
null
null
C(=O)O
Aromatic Heterocycle Formation
OtherReaction
26779edfcc2b370e3e3dc285e0fedfbcf04e6b6c7fd46f2674bab3f061a7b270
c12bf4e666f812d0e692aca3756678364265d1c8b3469e9563c84f9ed1df94d2
c1ccc(CCn2cnc3cnc4ccccc4c32)cc1
[C:1]-[C:2]-[NH;D2;+0:3]-[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1-[NH2;D1;+0:10]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[c:11]:[n;H0;D2;+0:10]:[c:9]2:[c:8]:[#7;a:7]:[c:6]:[c:5]:[c:4]:2:1
null
[]
null
null
null
null
Using the method of Example 31, 3-amino-4-[2-(phenyl)ethylamino]quinoline was reacted with triethyl orthoformate and formic acid to provide 1-[2-(phenyl)ethyl]-1H-imidazo[4,5-c]quinoline, m.p. 105°-108° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1nc[nH]c12
c1ccccc1.c1ccc2c(c1)ncc1nc[nH]c12
Other
C(=O)O
null
null
Nc1cnc2ccccc2c1NCCc1ccccc1>C(=O)O>c1ccc(CCn2cnc3cnc4ccccc4c32)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-2c24100fb43743379bf527993650331f
CCOC(C)(OCC)OCC.Nc1cnc2ccccc2c1NCc1ccccc1>>Cc1nc2cnc3ccccc3c2n1Cc1ccccc1.O
NC=1C=NC2=CC=CC=C2C1NCC1=CC=CC=C1.C(C)(OCC)(OCC)OCC>>O.C(C1=CC=CC=C1)N1C(=NC=2C=NC=3C=CC=CC3C21)C
CCO[C:2](OCC)([CH3:1])[O:22]CC.[NH2:3][c:4]1[cH:5][n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[c:13]1[NH:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1>>[CH3:1][c:2]1[n:3][c:4]2[cH:5][n:6][c:7]3[cH:8][cH:9][cH:10][cH:11][c:12]3[c:13]2[n:14]1[CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1.[OH2:22]
CCOC(C)(OCC)OCC.Nc1cnc2ccccc2c1NCc1ccccc1
Cc1nc2cnc3ccccc3c2n1Cc1ccccc1.O
null
null
C(C)(=O)O
Aromatic Heterocycle Formation
OtherReaction
af7d6de7ca5153ecd31a13d7075f2969261301df4b656bfec36bc67fd1ea176b
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc(Cn2cnc3cnc4ccccc4c32)cc1
C-C-O-[C;H0;D4;+0:1](-[C;D1;H3:2])(-O-C-C)-[O;H0;D2;+0:3]-C-C.[NH2;D1;+0:4]-[c:5]1:[c:6]:[#7;a:7]:[c:8]:[c:9]:[c:10]:1-[NH;D2;+0:11]-[C:12]-[c:13]>>[C;D1;H3:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:4]:[c:5]2:[c:6]:[#7;a:7]:[c:8]:[c:9]:[c:10]:2:[n;H0;D3;+0:11]:1-[C:12]-[c:13].[OH2;D0;+0:3]
null
[]
null
null
null
null
Using the method of Example 31, 3-amino-4-(benzylamino)quinoline (from Example 124, Part B) was reacted with triethyl orthoacetate and acetic acid to provide 1-benzyl-2-methyl-1H-imidazo[4,5-c]quinoline hydrate, m.p. 145°-147° C. Analysis: Calculated for C18H15N3 ·2.25H2O: % C, 68.9; % H, 6.3; % N, 13.4; Found: % C, 69...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
HO-
C(C)(=O)O
null
null
CCOC(C)(OCC)OCC.Nc1cnc2ccccc2c1NCc1ccccc1>C(C)(=O)O>Cc1nc2cnc3ccccc3c2n1Cc1ccccc1.O
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-cb431508c7dd457ab6337acbc87ef42d
N.OCCn1cnc2c(Cl)nc3ccccc3c21>>Nc1nc2ccccc2c2c1ncn2CCO
ClC1=NC=2C=CC=CC2C2=C1N=CN2CCO.N>>OCCN1C=NC=2C(=NC=3C=CC=CC3C21)N
[NH3:1].Cl[c:2]1[n:3][c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[c:10]2[c:11]1[n:12][cH:13][n:14]2[CH2:15][CH2:16][OH:17]>>[NH2:1][c:2]1[n:3][c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[c:10]2[c:11]1[n:12][cH:13][n:14]2[CH2:15][CH2:16][OH:17]
N.OCCn1cnc2c(Cl)nc3ccccc3c21
Nc1nc2ccccc2c2c1ncn2CCO
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
a67570e0a22d637a1d2a31207671ab3b6e569ccedb0b9b67428b6008b9e1da93
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c:5]2:[#7;a:6](-[C:7]):[c:8]:[#7;a:9]:[c:10]:2:1.[NH3;D0;+0:11]>>[C:7]-[#7;a:6]1:[c:8]:[#7;a:9]:[c:10]2:[c:5]:1:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:2-[NH2;D1;+0:11]
null
[]
null
null
null
null
A mixture of 4.0 g (0.016 mole) of 4-chloro-1-(2-hydroxyethyl)-1H-imidazo[4,5-c]quinoline (from Example 118) and 30 ml of 10% ammonia in methanol was heated in a steel bomb for 12 hours at 150° C. The resulting solid was separated from the cooled mixture by filtration, and was washed sequentially with water and methano...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2nc[nH]c12
HCl
CO
null
null
N.OCCn1cnc2c(Cl)nc3ccccc3c21>CO>Nc1nc2ccccc2c2c1ncn2CCO
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-97b456bb57504bd59428925f2a296995
CN.O=[N+]([O-])c1cnc2ccccc2c1O>>CNc1c([N+](=O)[O-])cnc2ccccc12
CN.OC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-].P(=O)(Cl)(Cl)Cl>>CNC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]
[CH3:1][NH2:2].O[c:3]1[c:4]([N+:5](=[O:6])[O-:7])[cH:8][n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]12>>[CH3:1][NH:2][c:3]1[c:4]([N+:5](=[O:6])[O-:7])[cH:8][n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]12
CN.O=[N+]([O-])c1cnc2ccccc2c1O
CNc1c([N+](=O)[O-])cnc2ccccc12
null
null
O.CN(C=O)C
Functional Group Addition
Reductive amination with alcohol
323be3a29db03987af5437147ca38f381a61d3758dc3e1e15c9bfbbe48d7afab
48d1b7679391da0e4d23024ff9a58734100ee909371b4065e4b5a1e4d85a7201
c1ccc2ncccc2c1
O-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C;D1;H3:10]-[NH2;D1;+0:11]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:11]-[C;D1;H3:10]
null
[]
null
null
null
null
To a solution of 5.7 g (0.030 mole) of 4-hydroxy-3-nitroquinoline in 50 ml of N,N-dimethylformamide was added 9.3 g (0.060 mole) of phosphorous oxychloride. The solution was heated on a steam bath for 5 minutes, then poured with stirring into 200 ml of 40% aqueous methylamine. The mixture was heated on a steam bath for...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HO-
O.CN(C=O)C
null
null
CN.O=[N+]([O-])c1cnc2ccccc2c1O>O.CN(C=O)C>CNc1c([N+](=O)[O-])cnc2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-b0d95afb09d243d89f5ffbf0df4d6ca8
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl.[OH-]>>CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.O
[OH-].[NH4+].P(=O)(Cl)(Cl)Cl.C(C(C)C)N1C=NC=2C=[N+](C=3C=CC=CC3C21)[O-]>>O.ClC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)C
[O-][n+:11]1[cH:9][c:8]2[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:18]2[c:17]2[c:12]1[cH:13][cH:14][cH:15][cH:16]2.O=P(Cl)(Cl)[Cl:10].[OH-:19]>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([Cl:10])[n:11][c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[c:18]12.[OH2:19]
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl.[OH-]
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.O
null
null
CN(C=O)C
Miscellaneous
OtherReaction
c5cfc3e69c2d1a66a8560034fe025f449600689a18546e68a564dc97632a28be
a48150e9dff88baab32dd83daf5ab089c597626e3c583c33a5868d8e1353c1ea
c1ccc2c(c1)ncc1nc[nH]c12
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[cH;D2;+0:7]:[n+;H0;D3:8](-[O-]):[c:9](:[c:10]):[c:11]:[c:12]:1:2.[OH-;D0:13]>>[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[c:12]:1:[c:11]:[c:9](:[c:10]):[n;H0;D2;+0:8]:[c;H0;D3;+0:7]:2-[Cl;H0;D1;+0:1].[OH2;D0;+0:13]
null
[]
20
CELSIUS
15
MINUTE
To a solution of 4.8 g (0.0311 mole) of phosphorus oxychloride in 20 ml of N,N-dimethylformamide was added in small portions 5.0 g (0.0207 mole) of 1-isobutyl-1H-imidazo[4,5-c]quinolin-5-oxide. The solution was stirred for 15 minutes at 20° C., then heated on a steam bath for 15 minutes. The solution was cooled to 20° ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2c(c1)[n+]cc1[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
Other
CN(C=O)C
20
0.25
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl.[OH-]>CN(C=O)C>CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.O
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-d6af7c98dd194e5db7be6f74241761d1
CCOC(C)(OCC)OCC.Nc1cnc2ccccc2c1NCCc1ccccc1>>Cc1nc2cnc3ccccc3c2n1CCc1ccccc1
NC=1C=NC2=CC=CC=C2C1NCCC1=CC=CC=C1.C(C)(OCC)(OCC)OCC>>CC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCC1=CC=CC=C1
CCO[C:2](OCC)(OCC)[CH3:1].[NH2:3][c:4]1[cH:5][n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[c:13]1[NH:14][CH2:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1>>[CH3:1][c:2]1[n:3][c:4]2[cH:5][n:6][c:7]3[cH:8][cH:9][cH:10][cH:11][c:12]3[c:13]2[n:14]1[CH2:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1
CCOC(C)(OCC)OCC.Nc1cnc2ccccc2c1NCCc1ccccc1
Cc1nc2cnc3ccccc3c2n1CCc1ccccc1
null
null
C(C)(=O)O
Aromatic Heterocycle Formation
OtherReaction
af7d6de7ca5153ecd31a13d7075f2969261301df4b656bfec36bc67fd1ea176b
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc(CCn2cnc3cnc4ccccc4c32)cc1
C-C-O-[C;H0;D4;+0:1](-[C;D1;H3:2])(-O-C-C)-O-C-C.[C:3]-[C:4]-[NH;D2;+0:5]-[c:6]1:[c:7]:[c:8]:[#7;a:9]:[c:10]:[c:11]:1-[NH2;D1;+0:12]>>[C:3]-[C:4]-[n;H0;D3;+0:5]1:[c:6]2:[c:7]:[c:8]:[#7;a:9]:[c:10]:[c:11]:2:[n;H0;D2;+0:12]:[c;H0;D3;+0:1]:1-[C;D1;H3:2]
null
[]
null
null
null
null
Using the method of Example 31, 3-amino-4-[2-(phenyl)ethylamino]quinoline (from Example 130, Part A) was reacted with triethyl orthoacetate and acetic acid to provide 2-methyl-1-[2-(phenyl)ethyl]-1H-imidazo[4,5-c]-quinoline. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
HO-
C(C)(=O)O
null
null
CCOC(C)(OCC)OCC.Nc1cnc2ccccc2c1NCCc1ccccc1>C(C)(=O)O>Cc1nc2cnc3ccccc3c2n1CCc1ccccc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-40c5db691dac434a8e856094f8e30b26
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.N>>CC(C)Cn1cnc2c(N)nc3ccccc3c21
ClC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)C.N>>C(C(C)C)N1C=NC=2C(=NC=3C=CC=CC3C21)N
Cl[c:9]1[c:8]2[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:18]2[c:17]2[c:12]([n:11]1)[cH:13][cH:14][cH:15][cH:16]2.[NH3:10]>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[c:18]12
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.N
CC(C)Cn1cnc2c(N)nc3ccccc3c21
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
c28f0ec61c908136ffb0a30dd77edf081d280d13023b48fbaccc360a51826dd0
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c:5]2:[#7;a:6](-[C:7]):[c:8]:[#7;a:9]:[c:10]:2:1.[NH3;D0;+0:11]>>[C:7]-[#7;a:6]1:[c:8]:[#7;a:9]:[c:10]2:[c:5]:1:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:2-[NH2;D1;+0:11]
null
[]
null
null
null
null
A mixture of 6.0 g (0.023 mole) of 4-chloro-1-isobuty-I-1H-imidazo[4,5-c]quinoline (from Example 77) and 30 ml of 20% ammonia in methanol was heated in a steel bomb for 18 hours at 150° C. The bomb was cooled, and the solid was separated by filtration, washed with methanol and recrystallized from N,N-dimethylformamide ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
HCl
CO
null
null
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.N>CO>CC(C)Cn1cnc2c(N)nc3ccccc3c21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-b76c5bba7f784ca49f6ef483068d4e3f
CCCCCCNc1c([N+](=O)[O-])cnc2ccccc12>>CCCCCCNc1c(N)cnc2ccccc12
C(CCCCC)NC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]>>NC=1C=NC2=CC=CC=C2C1NCCCCCC
O=[N+:10]([O-])[c:9]1[c:8]([NH:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])[c:18]2[c:13]([n:12][cH:11]1)[cH:14][cH:15][cH:16][cH:17]2>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][NH:7][c:8]1[c:9]([NH2:10])[cH:11][n:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12
CCCCCCNc1c([N+](=O)[O-])cnc2ccccc12
CCCCCCNc1c(N)cnc2ccccc12
null
[Pt]
C1(=CC=CC=C1)C
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2ncccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
null
[]
null
null
1.5
HOUR
To a solution of 22.5 g (0.0823 mole) of 4-(n-hexyl)amino-3-nitroquinoline in 300 ml of toluene was added about 1.0 g of 5% platinum on charcoal and the mixture was hydrogenated on a Paar apparatus for 1.5 hours. Filtration followed by evaporation in vacuo provided a residue of 3-amino-4-(n-hexyl)aminoquinoline as an o...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C1(=CC=CC=C1)C
null
1.5
CCCCCCNc1c([N+](=O)[O-])cnc2ccccc12>[Pt].C1(=CC=CC=C1)C>CCCCCCNc1c(N)cnc2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-d731061a926a478b9b411d4d4b43e710
CC(C)CN.O=[N+]([O-])c1cnc2ccccc2c1O>>CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12
C(C(C)C)N.Cl.C(C)N(CC)CC.P(=O)(Cl)(Cl)Cl.C(C(C)C)N.OC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]>>C(C(C)C)NC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]
[CH3:1][CH:2]([CH3:3])[CH2:4][NH2:5].O[c:6]1[c:7]([N+:8](=[O:9])[O-:10])[cH:11][n:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12>>[CH3:1][CH:2]([CH3:3])[CH2:4][NH:5][c:6]1[c:7]([N+:8](=[O:9])[O-:10])[cH:11][n:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12
CC(C)CN.O=[N+]([O-])c1cnc2ccccc2c1O
CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12
null
null
CN(C=O)C
Functional Group Addition
Reductive amination with alcohol
323be3a29db03987af5437147ca38f381a61d3758dc3e1e15c9bfbbe48d7afab
48d1b7679391da0e4d23024ff9a58734100ee909371b4065e4b5a1e4d85a7201
c1ccc2ncccc2c1
O-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
111.2
[{"value": 111.2, "product": "C(C(C)C)NC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To 50.0 g (0.269 mole) of 4-hydroxy-3-nitroquinoline in 300 ml of N,N-dimethylformamide in a 500 ml erlenmeyer flask was added, gradually, 44.3 g (0.2892 mole) of phosphorus oxychloride. The resulting mixture was heated on a steam bath for about 15 minutes, and was then poured onto ice with stirring. After neutralizati...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HO-
CN(C=O)C
null
null
CC(C)CN.O=[N+]([O-])c1cnc2ccccc2c1O>CN(C=O)C>CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-32844ea9b2634382ab9882881a5458d7
CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12>>CC(C)CNc1c(N)cnc2ccccc12
C(C(C)C)NC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]>>NC=1C=NC2=CC=CC=C2C1NCC(C)C
O=[N+:8]([O-])[c:7]1[c:6]([NH:5][CH2:4][CH:2]([CH3:1])[CH3:3])[c:16]2[c:11]([n:10][cH:9]1)[cH:12][cH:13][cH:14][cH:15]2>>[CH3:1][CH:2]([CH3:3])[CH2:4][NH:5][c:6]1[c:7]([NH2:8])[cH:9][n:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]12
CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12
CC(C)CNc1c(N)cnc2ccccc12
null
[Pt]
C1(=CC=CC=C1)C
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2ncccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
100.6
[{"value": 100.6, "product": "NC=1C=NC2=CC=CC=C2C1NCC(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Isobutylamino-3-nitroquinoline (31.5 g, 0.1284 moles) from Step (A) above, was dissolved in 300 ml of toluene, and about one g of platinum on charcoal was added thereto. The resulting mixture was hydrogenated on a Parr apparatus for one and one-half hours. The mixture was then heated and filtered. Toluene was removed...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C1(=CC=CC=C1)C
null
null
CC(C)CNc1c([N+](=O)[O-])cnc2ccccc12>[Pt].C1(=CC=CC=C1)C>CC(C)CNc1c(N)cnc2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-77406bcb46cf4afa95cd7512a1662d08
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl>>CC(C)Cn1cnc2c(Cl)nc3ccccc3c21
C(C(C)C)N1C=NC=2C=[N+](C=3C=CC=CC3C21)[O-].P(=O)(Cl)(Cl)Cl.[OH-].[NH4+]>>ClC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)C
[O-][n+:11]1[cH:9][c:8]2[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:18]2[c:17]2[c:12]1[cH:13][cH:14][cH:15][cH:16]2.O=P(Cl)(Cl)[Cl:10]>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([Cl:10])[n:11][c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[c:18]12
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21
null
null
CN(C=O)C
Miscellaneous
OtherReaction
c5cfc3e69c2d1a66a8560034fe025f449600689a18546e68a564dc97632a28be
a48150e9dff88baab32dd83daf5ab089c597626e3c583c33a5868d8e1353c1ea
c1ccc2c(c1)ncc1nc[nH]c12
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[cH;D2;+0:7]:[n+;H0;D3:8](-[O-]):[c:9](:[c:10]):[c:11]:[c:12]:1:2>>[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[c:12]:1:[c:11]:[c:9](:[c:10]):[n;H0;D2;+0:8]:[c;H0;D3;+0:7]:2-[Cl;H0;D1;+0:1]
89.9
[{"value": 89.9, "product": "ClC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
15
CELSIUS
30
MINUTE
To 40 ml of cold N,N-dimethylformamide (10°-20° C.) was added slowly 5.9 g (0.0385 mole) of phosphorus oxychloride with swirling, the temperature of the mixture being maintained at 10-20° C. 1-Isobutyl-1H-imidazo[4,5-c]quinolin-5-oxide (6.2 g; 0.0257 mole) from Step (C) above was added gradually with swirling and cooli...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2c(c1)[n+]cc1[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
HCl
CN(C=O)C
15
0.5
CC(C)Cn1cnc2c[n+]([O-])c3ccccc3c21.O=P(Cl)(Cl)Cl>CN(C=O)C>CC(C)Cn1cnc2c(Cl)nc3ccccc3c21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-9f8211210c6d4dbf81d1600cda775b83
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.N>>CC(C)Cn1cnc2c(N)nc3ccccc3c21
ClC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)C.N>>C(C(C)C)N1C=NC=2C(=NC=3C=CC=CC3C21)N
Cl[c:9]1[c:8]2[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:18]2[c:17]2[c:12]([n:11]1)[cH:13][cH:14][cH:15][cH:16]2.[NH3:10]>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[c:18]12
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.N
CC(C)Cn1cnc2c(N)nc3ccccc3c21
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
c28f0ec61c908136ffb0a30dd77edf081d280d13023b48fbaccc360a51826dd0
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c:5]2:[#7;a:6](-[C:7]):[c:8]:[#7;a:9]:[c:10]:2:1.[NH3;D0;+0:11]>>[C:7]-[#7;a:6]1:[c:8]:[#7;a:9]:[c:10]2:[c:5]:1:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:2-[NH2;D1;+0:11]
null
[]
null
null
8
HOUR
A mixture of 6.0 g (0.0231 mole) of 4-chloro-1-isobutyl-1H-imidazo[4,5-c]quinoline from Step (D) above and 30 ml of 20% ammonia in methanol was heated in a steel bomb for about 8 hours at about 145° C. The bomb was allowed to stand overnight at room temperature. The bomb was then cooled in an ice bath, and the solid th...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
HCl
CO
null
8
CC(C)Cn1cnc2c(Cl)nc3ccccc3c21.N>CO>CC(C)Cn1cnc2c(N)nc3ccccc3c21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-79e71bee98e74baf9f6c9abcace69231
CC(C)(O)CN.O=[N+]([O-])c1cnc2ccccc2c1Cl>>CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccccc12
ClC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-].OC(CN)(C)C>>OC(CNC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-])(C)C
[CH3:1][C:2]([CH3:3])([OH:4])[CH2:5][NH2:6].Cl[c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]12>>[CH3:1][C:2]([CH3:3])([OH:4])[CH2:5][NH:6][c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]12
CC(C)(O)CN.O=[N+]([O-])c1cnc2ccccc2c1Cl
CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccccc12
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2ncccc2c1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
null
[]
null
null
null
null
Using the method of Example 1, 4-chloro-3-nitroquinoline was reacted with 2-hydroxy-2-methylpropylamine to provide 4-(2-hydroxy-2-methylpropylamino)3-nitroquinoline, m.p. 234°-244° C. (dec.). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
null
null
null
CC(C)(O)CN.O=[N+]([O-])c1cnc2ccccc2c1Cl>>CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-688336cc55214556ac93ccfe0ea98ef2
CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccccc12>>CC(C)(O)CNc1c(N)cnc2ccccc12
OC(CNC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-])(C)C.C1(=CC=CC=C1)C>>NC=1C=NC2=CC=CC=C2C1NCC(C)(C)O
O=[N+:9]([O-])[c:8]1[c:7]([NH:6][CH2:5][C:2]([CH3:1])([CH3:3])[OH:4])[c:17]2[c:12]([n:11][cH:10]1)[cH:13][cH:14][cH:15][cH:16]2>>[CH3:1][C:2]([CH3:3])([OH:4])[CH2:5][NH:6][c:7]1[c:8]([NH2:9])[cH:10][n:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]12
CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccccc12
CC(C)(O)CNc1c(N)cnc2ccccc12
null
[Pt]
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2ncccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
null
[]
null
null
null
null
Using the method of Example 16, 7.0 g (0.027 mole) of 4-(2-hydroxy-2-methylpropylamino)-3-nitroquinoline, 1 g of platinum on charcoal, 200 ml of toluene and 150 ml of ethanol was hydrogenated on a Paar apparatus. The solution was filtered, then evaporated to dryness to provide 3-amino-4-(2-hydroxy-2-methylpropylamino)q...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C(C)O
null
null
CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccccc12>[Pt].C(C)O>CC(C)(O)CNc1c(N)cnc2ccccc12
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-37ae88eabedd477fbfe382c31767cfc2
CC(C)(O)Cn1cnc2c(Cl)nc3ccccc3c21.N>>CC(C)(O)Cn1cnc2c(N)nc3ccccc3c21
ClC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)(C)O.N>>NC1=NC=2C=CC=CC2C2=C1N=CN2CC(C)(C)O
Cl[c:10]1[c:9]2[n:8][cH:7][n:6]([CH2:5][C:2]([CH3:1])([CH3:3])[OH:4])[c:19]2[c:18]2[c:13]([n:12]1)[cH:14][cH:15][cH:16][cH:17]2.[NH3:11]>>[CH3:1][C:2]([CH3:3])([OH:4])[CH2:5][n:6]1[cH:7][n:8][c:9]2[c:10]([NH2:11])[n:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[c:19]12
CC(C)(O)Cn1cnc2c(Cl)nc3ccccc3c21.N
CC(C)(O)Cn1cnc2c(N)nc3ccccc3c21
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
c28f0ec61c908136ffb0a30dd77edf081d280d13023b48fbaccc360a51826dd0
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c:5]2:[#7;a:6](-[C:7]):[c:8]:[#7;a:9]:[c:10]:2:1.[NH3;D0;+0:11]>>[C:7]-[#7;a:6]1:[c:8]:[#7;a:9]:[c:10]2:[c:5]:1:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:2-[NH2;D1;+0:11]
null
[]
null
null
null
null
A mixture of 1.1 g (0.004 mole) of 4-chloro-1-(2-hydroxy-2-methylpropyl)-1H-imidazo[4,5-c]quinoline and 30 ml of 15 to 20% ammonia in methanol was heated at 150° to 160° C. for five hours in a bomb reactor. The mixture was filtered and the solid washed sequentially with methanol, ethyl acetate, water, and methanol then...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1nc2ccccc2c2nc[nH]c12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
HCl
CO
null
null
CC(C)(O)Cn1cnc2c(Cl)nc3ccccc3c21.N>CO>CC(C)(O)Cn1cnc2c(N)nc3ccccc3c21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-ccd81c7a01fc41eea9e96fd7b3fd7c67
CC(C)Cn1c(-c2ccccc2)nc2c(Cl)nc3ccccc3c21.CO.N>>CC(C)Cn1c(-c2ccccc2)nc2c(N)nc3ccccc3c21.O
ClC1=NC=2C=CC=CC2C2=C1N=C(N2CC(C)C)C2=CC=CC=C2.N.CO>>O.C(C(C)C)N1C(=NC=2C(=NC=3C=CC=CC3C21)N)C2=CC=CC=C2
Cl[c:15]1[c:14]2[n:13][c:6](-[c:7]3[cH:8][cH:9][cH:10][cH:11][cH:12]3)[n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:24]2[c:23]2[c:18]([n:17]1)[cH:19][cH:20][cH:21][cH:22]2.C[OH:25].[NH3:16]>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[c:6](-[c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[n:13][c:14]2[c:15]([NH2:16])[n:17][c:18]3[cH:19][cH:...
CC(C)Cn1c(-c2ccccc2)nc2c(Cl)nc3ccccc3c21.CO.N
CC(C)Cn1c(-c2ccccc2)nc2c(N)nc3ccccc3c21.O
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
8c8a5c893d886f8e242b67f9a3ad5148e87067796ba94f9095249c16bdc94ad8
152de3e76630e7985ec8784a0546cb68833650aaca34ad49d4293f11c3fa6912
c1ccc(-c2nc3cnc4ccccc4c3[nH]2)cc1
C-[OH;D1;+0:1].Cl-[c;H0;D3;+0:2]1:[#7;a:3]:[c:4]:[c:5]:[c:6]2:[#7;a:7](-[C:8]):[c:9]:[#7;a:10]:[c:11]:2:1.[NH3;D0;+0:12]>>[C:8]-[#7;a:7]1:[c:9]:[#7;a:10]:[c:11]2:[c:6]:1:[c:5]:[c:4]:[#7;a:3]:[c;H0;D3;+0:2]:2-[NH2;D1;+0:12].[OH2;D0;+0:1]
null
[]
null
null
null
null
A mixture of 5.6 g (0.016 mole) of 4-chloro-1-isobutyl-2-phenyl-1H-imidazo[4,5-c]quinoline and 30 ml of a 20% mixture of ammonia in methanol was placed in a metal bomb and heated at 145°-150° C. for about 6 hours. After cooling, the solid was separated by filtration, washed with methanol and dried to provide 3.8 g of c...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Methanol
Primary amine
c1nc2c(cnc3ccccc32)[nH]1
c1nc2cnc3ccccc3c2[nH]1
c1ccccc1.c1nc2cnc3ccccc3c2[nH]1
HCl
null
null
null
CC(C)Cn1c(-c2ccccc2)nc2c(Cl)nc3ccccc3c21.CO.N>>CC(C)Cn1c(-c2ccccc2)nc2c(N)nc3ccccc3c21.O
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-4558a0d0ae84408dbd0ef2b8670238d8
CNc1c(N)cnc2ccccc12.O=Cc1ccccc1>>Cn1c(-c2ccccc2)nc2cnc3ccccc3c21
NC=1C=NC2=CC=CC=C2C1NC.C(C1=CC=CC=C1)=O>>CN1C(=NC=2C=NC=3C=CC=CC3C21)C2=CC=CC=C2
[CH3:1][NH:2][c:20]1[c:11]([NH2:10])[cH:12][n:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]21.O=[CH:3][c:4]1[cH:5][cH:6][cH:7][cH:8][cH:9]1>>[CH3:1][n:2]1[c:3](-[c:4]2[cH:5][cH:6][cH:7][cH:8][cH:9]2)[n:10][c:11]2[cH:12][n:13][c:14]3[cH:15][cH:16][cH:17][cH:18][c:19]3[c:20]12
CNc1c(N)cnc2ccccc12.O=Cc1ccccc1
Cn1c(-c2ccccc2)nc2cnc3ccccc3c21
null
null
null
Aromatic Heterocycle Formation
OtherReaction
46c093c164e38091133c376b7b402743704aca08af9e6ec3245496a8ac99dc6d
102dc8cc7684c6225e704279ada61418fcb470f382f53c7127f5c8ad00fc07fc
c1ccc(-c2nc3cnc4ccccc4c3[nH]2)cc1
O=[CH;D2;+0:1]-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5]:[c:6].[C;D1;H3:7]-[NH;D2;+0:8]-[c:9]1:[c:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1-[NH2;D1;+0:15]>>[C;D1;H3:7]-[n;H0;D3;+0:8]1:[c:9]2:[c:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:2:[n;H0;D2;+0:15]:[c;H0;D3;+0:1]:1-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5]:[c:6]
null
[]
null
null
null
null
Following the general method of Example 195, Step B, 3-amino-4-(methylamino)quinoline was reacted with benzaldehyde to provide 1-methyl-2-phenyl-1H-imidazo[4,5-c]quinoline, melting point 168-170° C. Analysis: Calculated for C17H13N3 : % C, 78.7; % H, 5.1; % N, 16.2. Found: % C, 78.9; % H, 5.0; % N, 16.1. Conditions: Se...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2cnc3ccccc3c2[nH]1
c1ccccc1.c1nc2cnc3ccccc3c2[nH]1
HO-
null
null
null
CNc1c(N)cnc2ccccc12.O=Cc1ccccc1>>Cn1c(-c2ccccc2)nc2cnc3ccccc3c21
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-34c8435756eb44168d336df0c543e20d
CC(C)CNc1c(N)cnc2ccccc12.COc1ccc(C=O)cc1OC>>COc1ccc(-c2nc3cnc4ccccc4c3n2CC(C)C)cc1OC
NC=1C=NC2=CC=CC=C2C1NCC(C)C.C(C1=CC(OC)=C(OC)C=C1)=O>>COC=1C=C(C=CC1OC)C=1N(C2=C(C=NC=3C=CC=CC23)N1)CC(C)C
[NH2:8][c:9]1[cH:10][n:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[c:18]1[NH:19][CH2:20][CH:21]([CH3:22])[CH3:23].O=[CH:7][c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[c:25]([O:26][CH3:27])[cH:24]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[n:8][c:9]3[cH:10][n:11][c:12]4[cH:13][cH:14][cH:15][cH:16][c:17]4[c:18]3[n:19]2[CH2...
CC(C)CNc1c(N)cnc2ccccc12.COc1ccc(C=O)cc1OC
COc1ccc(-c2nc3cnc4ccccc4c3n2CC(C)C)cc1OC
null
null
null
Aromatic Heterocycle Formation
OtherReaction
93bb1b44f1d1432768c071e289ea08e6380da40bcdeccf4285629e70068050c1
102dc8cc7684c6225e704279ada61418fcb470f382f53c7127f5c8ad00fc07fc
c1ccc(-c2nc3cnc4ccccc4c3[nH]2)cc1
O=[CH;D2;+0:1]-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5]:[c:6].[C:7]-[C:8]-[NH;D2;+0:9]-[c:10]1:[c:11]:[c:12]:[#7;a:13]:[c:14]:[c:15]:1-[NH2;D1;+0:16]>>[C:7]-[C:8]-[n;H0;D3;+0:9]1:[c:10]2:[c:11]:[c:12]:[#7;a:13]:[c:14]:[c:15]:2:[n;H0;D2;+0:16]:[c;H0;D3;+0:1]:1-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5]:[c:6]
null
[]
null
null
null
null
Following the general method of Example 195, Step B, 3-amino-4-(isobutylamino)quinoline was reacted with veratraldehyde to provide 2-(3,4-dimethoxyphenyl)-1-isobutyl-1H-imidazo[4,5-c]quinoline, melting point 192°-199° C. Analysis: Calculated for C20H23N3O2 : % C, 73.1; % H, 6.4; % N, 11.6. Found: % C, 72.7; % H, 6.3; %...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1ccccc1.c1nc2c(cnc3ccccc32)[nH]1
HO-
null
null
null
CC(C)CNc1c(N)cnc2ccccc12.COc1ccc(C=O)cc1OC>>COc1ccc(-c2nc3cnc4ccccc4c3n2CC(C)C)cc1OC
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-1c55745b770e48968de56de9887cde31
CC(=O)Nc1ccc(CCCCOC(C)=O)cc1>>CC(=O)Nc1ccc(CCCCO)cc1
C(C)(=O)OCCCCC1=CC=C(C=C1)NC(C)=O.C([O-])([O-])=O.[K+].[K+]>>C(C)(=O)NC1=CC=C(C=C1)CCCCO
CC(=O)[O:13][CH2:12][CH2:11][CH2:10][CH2:9][c:8]1[cH:7][cH:6][c:5]([NH:4][C:2]([CH3:1])=[O:3])[cH:15][cH:14]1>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]([CH2:9][CH2:10][CH2:11][CH2:12][OH:13])[cH:14][cH:15]1
CC(=O)Nc1ccc(CCCCOC(C)=O)cc1
CC(=O)Nc1ccc(CCCCO)cc1
null
null
O.C(C)O
Reduction
Hydrolysis or Hydrogenolysis of Carboxylic Esters or Thioesters
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccccc1
C-C(=O)-[O;H0;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[OH;D1;+0:1]
null
[]
55
CELSIUS
null
null
To a solution of 19.3 g (0.077 mole) of acetic acid, 4-[4-(acetylamino)phenyl]butyl ester in 300 ml of ethanol, add a solution of 21 g potassium carbonate in 300 ml of water. Heat the resulting solution at 55° C. for 4 hrs. following the progress of the reaction by thin-layer chromatography on silica gel (acetonitrile:...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccccc1
HO-
O.C(C)O
55
null
CC(=O)Nc1ccc(CCCCOC(C)=O)cc1>O.C(C)O>CC(=O)Nc1ccc(CCCCO)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-0333de16236342b8b20d9c4d91eee625
CCCCCCCBr.Cc1nc(C)c(C)[nH]1>>CCCCCCCn1c(C)nc(C)c1C
O.[H-].[Na+].Cl.CC=1NC(=C(N1)C)C.C(CCCCCC)Br>>C(CCCCCC)N1C(=NC(=C1C)C)C
Br[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1].[nH:8]1[c:9]([CH3:10])[n:11][c:12]([CH3:13])[c:14]1[CH3:15]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][n:8]1[c:9]([CH3:10])[n:11][c:12]([CH3:13])[c:14]1[CH3:15]
CCCCCCCBr.Cc1nc(C)c(C)[nH]1
CCCCCCCn1c(C)nc(C)c1C
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
b9d84e1ee028da6e8c5d8924d45fbf8f3755d9adc2caf0035bd5ed7f30f5ee03
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
c1c[nH]cn1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[C;D1;H3:4]-[c:5]1:[#7;a:6]:[c:7](-[C;D1;H3:8]):[c:9](-[C;D1;H3:10]):[nH;D2;+0:11]:1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:11]1:[c:9](-[C;D1;H3:10]):[c:7](-[C;D1;H3:8]):[#7;a:6]:[c:5]:1-[C;D1;H3:4]
null
[]
0
CELSIUS
30
MINUTE
Dissolve 16.0 g (0.019 mole) of 2,4,5-trimethyl-1H-imidazole hydrochloride in 125 ml dry N,N-dimethylformamide and cool to 0° C. Add 8.75 g (0.218 mole) of sodium hydride (60%), stir at 0° C. for 30 minutes and then heat reaction mixture to 100° C. for one hour. Cool to 0° C. and then add 18.0 ml (0.114 mole) of n-hept...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1c[nH]cn1
c1c[nH]cn1
c1c[nH]cn1
HBr
CN(C=O)C
0
0.5
CCCCCCCBr.Cc1nc(C)c(C)[nH]1>CN(C=O)C>CCCCCCCn1c(C)nc(C)c1C
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-57b944a444a247edb173341c73d19415
BrC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=Cc1ccc(Cl)cc1>>C#Cc1ccc(Cl)cc1
CC(C)([O-])C.[K+].[Cl-].[NH4+].[Br-].BrC[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.CC(C)([O-])C.[K+].ClC1=CC=C(C=O)C=C1>>ClC1=CC=C(C=C1)C#C
Br[CH2:1][P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=[CH:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[cH:8][cH:9]1>>[CH:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[cH:8][cH:9]1
BrC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=Cc1ccc(Cl)cc1
C#Cc1ccc(Cl)cc1
null
null
O.C1CCOC1
Miscellaneous
OtherReaction
b5e69f6284ae9f6c52b1911e39a0a898004174961d6025d7bb8cb77cbd850106
308ec825ff187ec0e11eceb565511738e2dacb42c714ffa84b499d992753cbd1
c1ccccc1
Br-[CH2;D2;+0:1]-[P+](-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1.O=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[CH;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]
null
[]
-78
CELSIUS
2
HOUR
Dissolve 276.5 g (0.634 mole) of bromomethyltriphenyl phosphonium bromide in 1800 ml THF and cool to -78° C. Add 67.6 g (0.062 mole) potassium tert.-butoxide and stir at -78° C. for 2 hours. Add 89.12 g p-chlorobenzaldehyde in 200 ml THF to cold reaction mixture and stir for 30 minutes. Add 142.3 g potassium tert.-buto...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aldehyde
Alkyne
c1ccccc1.c1ccccc1.c1ccccc1
null
c1ccccc1
HBr
O.C1CCOC1
-78
2
BrC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=Cc1ccc(Cl)cc1>O.C1CCOC1>C#Cc1ccc(Cl)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-bdc533e715184965bbc0536d30ee978f
C#Cc1ccc(Cl)cc1.C1CO1>>OCCC#Cc1ccc(Cl)cc1
[Cl-].[NH4+].C(CCC)[Li].ClC1=CC=C(C=C1)C#C.C1CO1>>ClC1=CC=C(C=C1)C#CCCO
[CH:4]#[C:5][c:6]1[cH:7][cH:8][c:9]([Cl:10])[cH:11][cH:12]1.[O:1]1[CH2:2][CH2:3]1>>[OH:1][CH2:2][CH2:3][C:4]#[C:5][c:6]1[cH:7][cH:8][c:9]([Cl:10])[cH:11][cH:12]1
C#Cc1ccc(Cl)cc1.C1CO1
OCCC#Cc1ccc(Cl)cc1
null
null
C1CCOC1
C-C Coupling
OtherReaction
74881f120d30039dded129c43f3931fc5b61be5ec7ff7e68b1ee41afe1e0a524
47c0afae0bab7143ec21638567c860dc3df06c531350cee5b2c3bb02fce1440c
c1ccccc1
[CH;D1;+0:1]#[C:2]-[c:3].[C:4]1-[CH2;D2;+0:5]-[O;H0;D2;+0:6]-1>>[OH;D1;+0:6]-[C:4]-[CH2;D2;+0:5]-[C;H0;D2;+0:1]#[C:2]-[c:3]
null
[]
-78
CELSIUS
2
HOUR
Dissolve 14.2 g (0.104 mole) of 1-chloro-4-ethynylbenzene in 35 ml dry THF and cool to -78° C. Add 49 ml butyl lithium to cold reaction mixture and allow to warm to room temperature for 2 hours. After 2 hours, cool to -78° C. and the add 5.8 ml (0.114 mole) ethylene oxide in 20 ml THF. Allow to warm to room temperature...
10.6084/m9.figshare.5104873.v1
null
Ether.Alkyne
Primary alcohol.Alkyne
C1CO1
null
c1ccccc1
null
C1CCOC1
-78
2
C#Cc1ccc(Cl)cc1.C1CO1>C1CCOC1>OCCC#Cc1ccc(Cl)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-1c4e4b4ca92940e9b18a794c32368b52
Cc1ccc(S(=O)(=O)Cl)cc1>>Cc1ccc(S(=O)(=O)[O-])cc1
ClC1=CC=C(C=C1)C#CCCO.C1(=CC=C(C=C1)S(=O)(=O)Cl)C.C(C)OCC>>ClC1=CC=C(C=C1)C#CCCO.CC1=CC=C(C=C1)S(=O)(=O)[O-]
Cl[S:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:11][cH:10]1)(=[O:7])=[O:8]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[O-:9])[cH:10][cH:11]1
Cc1ccc(S(=O)(=O)Cl)cc1
Cc1ccc(S(=O)(=O)[O-])cc1
null
null
N1=CC=CC=C1
Functional Group Interconversion
OtherReaction
0cd2ed4c6a94f21490c2adf2b68d468bae5848a2a7182f1ca312bdc9820ddd3f
fcd366d2a12b9f2b1304281b4b55e60873460be0844fd3f482f05b099eb21cf7
c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]>>[O;-;D1;H0:7]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
null
[]
0
CELSIUS
1
HOUR
Dissolve 13.3 g (0.0736 mole) of 4-(4-chlorophenyl)-3-butyn-1-ol in 70 ml pyridine and cool to 0° C. Add 16 g (0.0837 mole) of p-toluenesulfonyl chloride and stir in ice bath for one hour. Store in freezer over night. Add 200 ml diethyl ether and then wash with 3×150 ml 1N hydrochloric acid. The organic layer is then w...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Sulfonyl halide
Tosylate
null
null
c1ccccc1
null
N1=CC=CC=C1
0
1
Cc1ccc(S(=O)(=O)Cl)cc1>N1=CC=CC=C1>Cc1ccc(S(=O)(=O)[O-])cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-e58ccd8a18b34601959a020e8d497689
CS(=O)(=O)Cl.CS(=O)(=O)Cl.Nc1ccc(CCCCO)cc1>>CS(=O)(=O)Nc1ccc(CCCCOS(C)(=O)=O)cc1
CS(=O)(=O)Cl.NC1=CC=C(C=C1)CCCCO.CS(=O)(=O)Cl>>CS(=O)(=O)OCCCCC1=CC=C(C=C1)NS(=O)(=O)C
Cl[S:2]([CH3:1])(=[O:3])=[O:4].Cl[S:15]([CH3:16])(=[O:17])=[O:18].[NH2:5][c:6]1[cH:7][cH:8][c:9]([CH2:10][CH2:11][CH2:12][CH2:13][OH:14])[cH:19][cH:20]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][c:6]1[cH:7][cH:8][c:9]([CH2:10][CH2:11][CH2:12][CH2:13][O:14][S:15]([CH3:16])(=[O:17])=[O:18])[cH:19][cH:20]1
CS(=O)(=O)Cl.CS(=O)(=O)Cl.Nc1ccc(CCCCO)cc1
CS(=O)(=O)Nc1ccc(CCCCOS(C)(=O)=O)cc1
null
null
N1=CC=CC=C1
Acylation
OtherReaction
b2bf6220584234f1bd19047ee82945b25f43600c7ad23e864d53425aab806ad7
6c124ade914d189e6ed09bfe0a6c1651505ee2fd7e35365d194d1b93a5b77eb7
c1ccccc1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].Cl-[S;H0;D4;+0:5](-[C;D1;H3:6])(=[O;D1;H0:7])=[O;D1;H0:8].[C:9]-[C:10]-[OH;D1;+0:11].[NH2;D1;+0:12]-[c:13](:[c:14]):[c:15]>>[C;D1;H3:2]-[S;H0;D4;+0:1](=[O;D1;H0:3])(=[O;D1;H0:4])-[NH;D2;+0:12]-[c:13](:[c:14]):[c:15].[C:9]-[C:10]-[O;H0;D2;+0:11]-[S;H0;D4;+0:5](-[...
null
[]
-10
CELSIUS
2
DAY
9.25 g (0.056 mole) 4-aminobenzenebutanol is dissolved in 100 ml pyridine and the solution is cooled to ca. -10° C. 17.33 ml (25.65 g) (0.244 mole) methanesulfonyl chloride is added dropwise with vigorous stirring at a rate such that the methanesulfonyl chloride is added, the reaction mixture is left in the freezer for...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Primary amine.Sulfonyl halide.Sulfonyl halide
Sulfonamide.Mesylate
null
null
c1ccccc1
HCl
N1=CC=CC=C1
-10
48
CS(=O)(=O)Cl.CS(=O)(=O)Cl.Nc1ccc(CCCCO)cc1>N1=CC=CC=C1>CS(=O)(=O)Nc1ccc(CCCCOS(C)(=O)=O)cc1
ord_dataset-c34472859da14a81bfe0f74e60f15c43
ord-eb0e73cb164b48d4ba41188c18c754fc
Cl.Nc1cccc(Cl)c1Cl>>N#[N+]c1cccc(Cl)c1Cl.[Cl-]
N(=O)[O-].[Na+].ClC1=C(N)C=CC=C1Cl.Cl>>[Cl-].ClC1=C(C=CC=C1Cl)[N+]#N
[ClH:11].[NH2:2][c:3]1[cH:4][cH:5][cH:6][c:7]([Cl:8])[c:9]1[Cl:10]>>[N:1]#[N+:2][c:3]1[cH:4][cH:5][cH:6][c:7]([Cl:8])[c:9]1[Cl:10].[Cl-:11]
Cl.Nc1cccc(Cl)c1Cl
N#[N+]c1cccc(Cl)c1Cl.[Cl-]
null
null
O
Functional Group Interconversion
OtherReaction
4b9613e8eb03ba0ca635945a60e7b18985445e9967460b2f7cd3bfa7398bb2a3
ca5105ff0b33557e585dc54e7cfdd7fa7df4e7f9c3edc13b706f4674b75a100e
c1ccccc1
[ClH;D0;+0:1].[NH2;D1;+0:2]-[c:3](:[c:4]):[c:5]>>[Cl-;H0;D0:1].[N;D1;H0:6]#[N+;H0;D2:2]-[c:3](:[c:4]):[c:5]
null
[]
null
null
5
MINUTE
To a suspension of 25 g (0.15 mole) 2,3-dichloroaniline in 16 ml H2O, add 39 ml (0.46 mole) concentrated HCl. Stir the mixture at room temperature for about five minutes. Cool the mixture to -5° to 0° C. and add dropwise a solution of 11 g (0.16 mole) NaNO2 in 30 ml H2O. Stir the resulting solution at -5° to 0° C. for ...
10.6084/m9.figshare.5104873.v1
null
Primary amine
null
null
null
c1ccccc1
null
O
null
0.083333
Cl.Nc1cccc(Cl)c1Cl>O>N#[N+]c1cccc(Cl)c1Cl.[Cl-]