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large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
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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
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float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
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large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ec77dfb64e5b43ed8c980fa971400be6
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)OC>>CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)O
[OH-].[Na+].COC(=O)C1=C(N=C2N1N=C(C=C2C2=C(C=C(C=C2)C)C)C)CC>>CC1=C(C=CC(=C1)C)C=1C=2N(N=C(C1)C)C(=C(N2)CC)C(=O)O
C[O:23][C:21]([c:20]1[c:3]([CH2:2][CH3:1])[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][c:16]([CH3:17])[n:18][n:19]21)=[O:22]>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][c:16]([CH3:17])[n:18][n:19]2[c:20]1[C:21](=[O:22])[OH...
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)OC
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)O
null
null
C(C)O
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(-c2ccnn3ccnc23)cc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4](:[#7;a:5]:[#7;a:6]):[c:7]:[#7;a:8]>>[#7;a:6]:[#7;a:5]:[c:4](-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]):[c:7]:[#7;a:8]
null
[]
null
null
null
null
A 5N aqueous sodium hydroxide solution (20 mL) was added to a solution of the resulting 8-(2,4-dimethylphenyl)-2-ethyl-6-methylimidazo[1,2-b]pyridazin-3-carboxylic acid methyl ester in ethanol (100 mL), and the mixture was heated under reflux for 3 hours. The reaction mixture was evaporated as it was. Water was added t...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1cnn2ccnc2c1
Other
C(C)O
null
null
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)OC>C(C)O>CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f219c0459560454a888fc84392da9705
CC(C)(C)O.CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)O.[N-]=[N+]=Nc1[pH]cc(-c2ccccc2)c1-c1ccccc1>>CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1NC(=O)OC(C)(C)C
O.C(C)N(CC)CC.C(C)(C)(C)O.C1(=CC=CC=C1)C=1C(=C(PC1)N=[N+]=[N-])C1=CC=CC=C1.CC1=C(C=CC(=C1)C)C=1C=2N(N=C(C1)C)C(=C(N2)CC)C(=O)O>>CC1=C(C=CC(=C1)C)C=1C=2N(N=C(C1)C)C(=C(N2)CC)NC(OC(C)(C)C)=O
[OH:24][C:25]([CH3:26])([CH3:27])[CH3:28].O[C:22]([c:20]1[c:3]([CH2:2][CH3:1])[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][c:16]([CH3:17])[n:18][n:19]21)=[O:23].[N-]=[N+]=[N:21]c1[pH]cc(-c2ccccc2)c1-c1ccccc1>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[...
CC(C)(C)O.CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)O.[N-]=[N+]=Nc1[pH]cc(-c2ccccc2)c1-c1ccccc1
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1NC(=O)OC(C)(C)C
null
null
C1(=CC=CC=C1)C
Protection
OtherReaction
955039b1b29a15c4df8b7152053c3a2b3b9a3404b0b3f43d655c58d05cc605d1
b944663b5278c281edc6c72611c69e4309c3f5728dcd63d51413085e18c1d2e7
c1ccc(-c2ccnn3ccnc23)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:3]1:[#7;a:4](:[#7;a:5]:[c:6]):[c:7](:[c:8]):[#7;a:9]:[c:10]:1-[C:11].[C;D1;H3:12]-[C:13](-[C;D1;H3:14])(-[C;D1;H3:15])-[OH;D1;+0:16].[N-]=[N+]=[N;H0;D2;+0:17]-c1:[pH]:c:c(-c2:c:c:c:c:c:2):c:1-c1:c:c:c:c:c:1>>[C:11]-[c:10]1:[#7;a:9]:[c:7](:[c:8]):[#7;a:4](:[#7;a:5]:[c:6]):[c;H0...
null
[]
140
CELSIUS
null
null
Triethylamine (20 mL), tert-butyl alcohol (30 mL) and diphenylphospholylazide (1.95 mL, 9.05 mmol) were added to a solution of the resulting 8-(2,4-dimethylphenyl)-2-ethyl-6-methylimidazo[1,2-b]pyridazine-3-carboxylic acid (2.8 g, 9.05 mmol) in toluene (40 mL), and the mixture was heated at 140° C. for 6 hours. Water w...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Azide.Tertiary alcohol
Carbamic ester.Ether.Boc
c1cnn2ccnc2c1.c1cc[pH]c1.c1ccccc1.c1ccccc1
c1cnn2ccnc2c1
c1ccccc1.c1cnn2ccnc2c1
HO-
C1(=CC=CC=C1)C
140
null
CC(C)(C)O.CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1C(=O)O.[N-]=[N+]=Nc1[pH]cc(-c2ccccc2)c1-c1ccccc1>C1(=CC=CC=C1)C>CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1NC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6c4d5a1da9ca485899cb2ced4ee490a0
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1NC(=O)OC(C)(C)C>>CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1N
Cl.C(C)(=O)OCC.CC1=C(C=CC(=C1)C)C=1C=2N(N=C(C1)C)C(=C(N2)CC)NC(OC(C)(C)C)=O.[OH-].[Na+]>>CC1=C(C=CC(=C1)C)C=1C=2N(N=C(C1)C)C(=C(N2)CC)N
CC(C)(C)OC(=O)[NH:21][c:20]1[c:3]([CH2:2][CH3:1])[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][c:16]([CH3:17])[n:18][n:19]21>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][c:16]([CH3:17])[n:18][n:19]2[c:20]1[NH2:21]
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1NC(=O)OC(C)(C)C
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1N
null
null
C(C)(=O)OCC
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc(-c2ccnn3ccnc23)cc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[c:2]1:[#7;a:3](:[#7;a:4]:[c:5]):[c:6]:[#7;a:7]:[c:8]:1-[C:9]>>[C:9]-[c:8]1:[#7;a:7]:[c:6]:[#7;a:3](:[#7;a:4]:[c:5]):[c:2]:1-[NH2;D1;+0:1]
null
[]
null
null
14
HOUR
4N hydrochloric acid/ethyl acetate (30 mL) was added to a solution of the resulting tert-butyl N-[8-(2,4-dimethylphenyl)-2-ethyl-6-methylimidazo[1,2-b]pyridazin-3-yl]carbamate in ethyl acetate (10 mL), and the mixture was stirred at room temperature for 14 hours. The mixture was neutralized by adding 5N aqueous sodium ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1cnn2ccnc2c1
HO-
C(C)(=O)OCC
null
14
CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1NC(=O)OC(C)(C)C>C(C)(=O)OCC>CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-99953881eaed4d98867e50172ed72367
CC(=O)O.CC(=O)O[BH-](OC(C)=O)OC(C)=O.CCC=O.CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1N>>CCCN(CCC)c1c(CC)nc2c(-c3ccc(C)cc3C)cc(C)nn12
C(C)(=O)O.C(CC)=O.CC1=C(C=CC(=C1)C)C=1C=2N(N=C(C1)C)C(=C(N2)CC)N.C(C)(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+]>>CC1=C(C=CC(=C1)C)C=1C=2N(N=C(C1)C)C(=C(N2)CC)N(CCC)CCC
O=[C:5](O)[CH3:6].CC(=O)O[BH-](OC(C)=O)OC(=O)[CH3:7].O=[CH:3][CH2:2][CH3:1].[NH2:4][c:8]1[c:9]([CH2:10][CH3:11])[n:12][c:13]2[c:14](-[c:15]3[cH:16][cH:17][c:18]([CH3:19])[cH:20][c:21]3[CH3:22])[cH:23][c:24]([CH3:25])[n:26][n:27]12>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7])[c:8]1[c:9]([CH2:10][CH3:11])[n:12][c:1...
CC(=O)O.CC(=O)O[BH-](OC(C)=O)OC(C)=O.CCC=O.CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1N
CCCN(CCC)c1c(CC)nc2c(-c3ccc(C)cc3C)cc(C)nn12
null
null
ClCCl.O
Heteroatom Alkylation and Arylation
OtherReaction
72e9da2aba1d8936b94244127c9bab45cbdbdb9e71f57cb28565a139dcef7a1d
996df106b620b728ac5024cde06f3dbfda15a09e51d5e7ab9b342c86c263d13f
c1ccc(-c2ccnn3ccnc23)cc1
C-C(=O)-O-[BH-](-O-C(-C)=O)-O-C(=O)-[CH3;D1;+0:1].O-[C;H0;D3;+0:2](=O)-[CH3;D1;+0:3].O=[CH;D2;+0:4]-[C:5]-[C;D1;H3:6].[C:7]-[c:8]1:[#7;a:9]:[c:10]:[#7;a:11](:[#7;a:12]:[c:13]):[c:14]:1-[NH2;D1;+0:15]>>[C:7]-[c:8]1:[#7;a:9]:[c:10]:[#7;a:11](:[#7;a:12]:[c:13]):[c:14]:1-[N;H0;D3;+0:15](-[CH2;D2;+0:4]-[C:5]-[C;D1;H3:6])-[C...
null
[]
null
null
10
MINUTE
Propionaldehyde (3.26 mL, 45.25 mmol) was added to a solution of the resulting 8-(2,4-dimethylphenyl)-2-ethyl-6-methylimidazo[1,2-b]pyridazin-3-amine (9.05 mmol) in dichloromethane (60 mL), and the mixture was stirred at room temperature for 10 minutes. Sodium triacetoxyborohydride (5.75 g, 27.15 mmol) was gradually ad...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Carboxylic acid.Primary amine
Tertiary amine
null
null
c1ccccc1.c1cnn2ccnc2c1
HO-.B
ClCCl.O
null
0.166667
CC(=O)O.CC(=O)O[BH-](OC(C)=O)OC(C)=O.CCC=O.CCc1nc2c(-c3ccc(C)cc3C)cc(C)nn2c1N>ClCCl.O>CCCN(CCC)c1c(CC)nc2c(-c3ccc(C)cc3C)cc(C)nn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2a6d8a1afc0e40998dc141f77e43efb9
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)OC>>CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)O
[OH-].[Na+].CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)C(=O)OC.Cl>>CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)C(=O)O
C[O:22][C:20]([c:19]1[c:3]([CH2:2][CH3:1])[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][cH:16][n:17][n:18]21)=[O:21]>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][cH:16][n:17][n:18]2[c:19]1[C:20](=[O:21])[OH:22]
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)OC
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)O
null
null
C(C)O
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(-c2ccnn3ccnc23)cc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4](:[#7;a:5]:[#7;a:6]):[c:7]:[#7;a:8]>>[#7;a:6]:[#7;a:5]:[c:4](-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]):[c:7]:[#7;a:8]
null
[]
null
null
null
null
A 5N aqueous sodium hydroxide solution (0.603 mL, 3.0 mmol) was added to a solution of methyl 8-(2,4-dimethylphenyl)-2-ethylimidazo[1,2-b]pyridazine-3-carboxylate (373 mg, 1.20 mmol) in ethanol (15 mL), and the mixture was heated under reflux for 1 hour. 5N hydrochloric acid (0.603 mL) was added thereto under ice-cooli...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1cnn2ccnc2c1
Other
C(C)O
null
null
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)OC>C(C)O>CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cfc37113527a4f9495b9846ad564c536
CC(C)(C)O.CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)O.[N-]=[N+]=Nc1[pH]cc(-c2ccccc2)c1-c1ccccc1>>CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1NC(=O)OC(C)(C)C
C(C)N(CC)CC.C(C)(C)(C)O.C1(=CC=CC=C1)C=1C(=C(PC1)N=[N+]=[N-])C1=CC=CC=C1.CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)C(=O)O.O>>CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)NC(OC(C)(C)C)=O
[OH:23][C:24]([CH3:25])([CH3:26])[CH3:27].O[C:21]([c:19]1[c:3]([CH2:2][CH3:1])[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][cH:16][n:17][n:18]21)=[O:22].[N-]=[N+]=[N:20]c1[pH]cc(-c2ccccc2)c1-c1ccccc1>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:...
CC(C)(C)O.CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)O.[N-]=[N+]=Nc1[pH]cc(-c2ccccc2)c1-c1ccccc1
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1NC(=O)OC(C)(C)C
null
null
C1(=CC=CC=C1)C
Protection
OtherReaction
955039b1b29a15c4df8b7152053c3a2b3b9a3404b0b3f43d655c58d05cc605d1
b944663b5278c281edc6c72611c69e4309c3f5728dcd63d51413085e18c1d2e7
c1ccc(-c2ccnn3ccnc23)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:3]1:[#7;a:4](:[#7;a:5]:[c:6]):[c:7](:[c:8]):[#7;a:9]:[c:10]:1-[C:11].[C;D1;H3:12]-[C:13](-[C;D1;H3:14])(-[C;D1;H3:15])-[OH;D1;+0:16].[N-]=[N+]=[N;H0;D2;+0:17]-c1:[pH]:c:c(-c2:c:c:c:c:c:2):c:1-c1:c:c:c:c:c:1>>[C:11]-[c:10]1:[#7;a:9]:[c:7](:[c:8]):[#7;a:4](:[#7;a:5]:[c:6]):[c;H0...
null
[]
110
CELSIUS
null
null
Triethylamine (0.202 mL, 1.4 mmol), t-butyl alcohol (5 mL) and diphenylphospholylazide (0.26 mL, 1.2 mmol) were added to a solution of the crude 8-(2,4-dimethylphenyl)-2-ethylimidazo[1,2-b]pyridazine-3-carboxylic acid (1.206 mmol) in toluene (10 mL), and the mixture was heated at 90° C. for 1 hour and 110° C. for 4 hou...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Azide.Tertiary alcohol
Carbamic ester.Ether.Boc
c1cnn2ccnc2c1.c1cc[pH]c1.c1ccccc1.c1ccccc1
c1cnn2ccnc2c1
c1ccccc1.c1cnn2ccnc2c1
HO-
C1(=CC=CC=C1)C
110
null
CC(C)(C)O.CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1C(=O)O.[N-]=[N+]=Nc1[pH]cc(-c2ccccc2)c1-c1ccccc1>C1(=CC=CC=C1)C>CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1NC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d97d971ddf644182ba53ba7ae07aaca8
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1NC(=O)OC(C)(C)C>>CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1N
Cl.C(C)(=O)OCC.CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)NC(OC(C)(C)C)=O.[OH-].[Na+]>>CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)N
CC(C)(C)OC(=O)[NH:20][c:19]1[c:3]([CH2:2][CH3:1])[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][cH:16][n:17][n:18]21>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][c:10]([CH3:11])[cH:12][c:13]3[CH3:14])[cH:15][cH:16][n:17][n:18]2[c:19]1[NH2:20]
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1NC(=O)OC(C)(C)C
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1N
null
null
C(C)(=O)OCC
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc(-c2ccnn3ccnc23)cc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[c:2]1:[#7;a:3](:[#7;a:4]:[c:5]):[c:6]:[#7;a:7]:[c:8]:1-[C:9]>>[C:9]-[c:8]1:[#7;a:7]:[c:6]:[#7;a:3](:[#7;a:4]:[c:5]):[c:2]:1-[NH2;D1;+0:1]
null
[]
null
null
15
HOUR
4N hydrochloric acid/ethyl acetate (15 mL) was added to a solution of the crude tert-butyl N-[8-(2,4-dimethylphenyl)-2-ethylimidazo[1,2-b]pyridazin-3-yl]carbamate in ethyl acetate (5 mL), and the mixture was stirred at room temperature for 15 hours. The mixture was neutralized by adding a 5N aqueous sodium hydroxide so...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1cnn2ccnc2c1
HO-
C(C)(=O)OCC
null
15
CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1NC(=O)OC(C)(C)C>C(C)(=O)OCC>CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f4ed6574379d403ca88d1259381799ea
C1CCOC1.CCC=O.CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1N>>CCCN(CCC)c1c(CC)nc2c(-c3ccc(C)cc3C)ccnn12
[BH4-].[Na+].C(CC)=O.S(O)(O)(=O)=O.CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)N.O1CCCC1.[OH-].[Na+]>>CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)N(CCC)CCC
C1O[CH2:6][CH2:5][CH2:7]1.O=[CH:3][CH2:2][CH3:1].[NH2:4][c:8]1[c:9]([CH2:10][CH3:11])[n:12][c:13]2[c:14](-[c:15]3[cH:16][cH:17][c:18]([CH3:19])[cH:20][c:21]3[CH3:22])[cH:23][cH:24][n:25][n:26]12>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7])[c:8]1[c:9]([CH2:10][CH3:11])[n:12][c:13]2[c:14](-[c:15]3[cH:16][cH:17][c:1...
C1CCOC1.CCC=O.CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1N
CCCN(CCC)c1c(CC)nc2c(-c3ccc(C)cc3C)ccnn12
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
6d53ba521f8dd859a1d027aff20a1f30229be42b36780b5882e61533b2cc295e
df535931b8059d394937514de5b7d3a229014cb8b85d7d4618a05bc841c21364
c1ccc(-c2ccnn3ccnc23)cc1
C1-O-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[CH2;D2;+0:3]-1.O=[CH;D2;+0:4]-[C:5]-[C;D1;H3:6].[C:7]-[c:8]1:[#7;a:9]:[c:10]:[#7;a:11](:[#7;a:12]:[c:13]):[c:14]:1-[NH2;D1;+0:15]>>[C:7]-[c:8]1:[#7;a:9]:[c:10]:[#7;a:11](:[#7;a:12]:[c:13]):[c:14]:1-[N;H0;D3;+0:15](-[CH2;D2;+0:4]-[C:5]-[C;D1;H3:6])-[CH2;D2;+0:2]-[CH2;D2;+0:1]-[CH3;D1;+0...
10
[{"value": 10.0, "product": "CC1=C(C=CC(=C1)C)C=1C=2N(N=CC1)C(=C(N2)CC)N(CCC)CCC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Propionaldehyde (0.435 mL, 6.0 mmol) and 3M sulfuric acid (2.01 mL, 6.0 mmol) were added to a solution of the crude 8-(2,4-dimethylphenyl)-2-ethylimidazo[1,2-b]pyridazin-3-amine (1.2 mmol) in tetrahydrofuran (10 mL) under ice-cooling, and sodium borohydride (182 mg, 4.8 mmol) was gradually added at the same temperature...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ether.Primary amine
Tertiary amine
C1CCOC1
null
c1ccccc1.c1cnn2ccnc2c1
HO-
O
null
0.5
C1CCOC1.CCC=O.CCc1nc2c(-c3ccc(C)cc3C)ccnn2c1N>O>CCCN(CCC)c1c(CC)nc2c(-c3ccc(C)cc3C)ccnn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-77c70f7d10ab4f73bd20ef27a44e65e9
CCCN(CCC)c1c(SC)nc2c(Br)cc(C)cn12.OB(O)c1ccc(Cl)cc1Cl>>CCCN(CCC)c1c(SC)nc2c(-c3ccc(Cl)cc3Cl)cc(C)cn12
BrC=1C=2N(C=C(C1)C)C(=C(N2)SC)N(CCC)CCC.ClC1=C(C=CC(=C1)Cl)B(O)O.O.O.O.O.O.O.O.O.[OH-].[Ba+2].[OH-]>>ClC1=C(C=CC(=C1)Cl)C=1C=2N(C=C(C1)C)C(=C(N2)SC)N(CCC)CCC
Br[c:14]1[c:13]2[n:12][c:9]([S:10][CH3:11])[c:8]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH2:6][CH3:7])[n:27]2[cH:26][c:24]([CH3:25])[cH:23]1.OB(O)[c:15]1[cH:16][cH:17][c:18]([Cl:19])[cH:20][c:21]1[Cl:22]>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][CH3:7])[c:8]1[c:9]([S:10][CH3:11])[n:12][c:13]2[c:14](-[c:15]3[cH:16][cH:17]...
CCCN(CCC)c1c(SC)nc2c(Br)cc(C)cn12.OB(O)c1ccc(Cl)cc1Cl
CCCN(CCC)c1c(SC)nc2c(-c3ccc(Cl)cc3Cl)cc(C)cn12
null
null
O.COCCOC
C-C Coupling
Suzuki coupling with boronic acids
6d2f92e38cbc7faf246cda8a4b8669001b5c18f23ff87160bd75535916dab019
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cccn3ccnc23)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]2:[c:6]:[c:7]:[#7;a:8]:[c:9]:2:1.O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13](-[Cl;D1;H0:14]):[c:15]>>[Cl;D1;H0:14]-[c:13](:[c:15]):[c;H0;D3;+0:10](-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]2:[c:6]:[c:7]:[#7;a:8]:[c:9]:2:1):[c:11]:[c:12]
72.5
[{"value": 72.5, "product": "ClC1=C(C=CC(=C1)Cl)C=1C=2N(C=C(C1)C)C(=C(N2)SC)N(CCC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
N-[8-Bromo-6-methyl-2-(methylsulfanyl)imidazo[1,2-a]pyridin-3-yl]-N,N-dipropylamine (50 mg) was dissolved in a mixed solvent of 1,2-dimethoxyethane (6 mL) and water (1 mL). 2,4-Dichlorobenzeneboronic acid (53 mg), barium hydroxide octahydrate (88 mg) and tetrakistriphenylphosphine palladium complex (16 mg) were added t...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccn2ccnc2c1.c1ccccc1
c1ccccc1.c1ccn2ccnc2c1
c1ccccc1.c1ccn2ccnc2c1
HBr.B
O.COCCOC
null
null
CCCN(CCC)c1c(SC)nc2c(Br)cc(C)cn12.OB(O)c1ccc(Cl)cc1Cl>O.COCCOC>CCCN(CCC)c1c(SC)nc2c(-c3ccc(Cl)cc3Cl)cc(C)cn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-453e93fc712446deb887ec2ae8b507a1
CCCN(CC1CC1)c1c(SC)nc2c(-c3ccc(OC)cc3Cl)nccn12.O=C(OO)c1cccc(Cl)c1>>CCCN(CC1CC1)c1c(S(C)=O)nc2c(-c3ccc(OC)cc3Cl)nccn12
ClC1=CC(=CC=C1)C(=O)OO.ClC1=C(C=CC(=C1)OC)C=1C=2N(C=CN1)C(=C(N2)SC)N(CCC)CC2CC2.S(=S)(=O)([O-])[O-].[Na+].[Na+].C([O-])(O)=O.[Na+]>>ClC1=C(C=CC(=C1)OC)C=1C=2N(C=CN1)C(=C(N2)S(=O)C)N(CCC)CC2CC2
[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH:6]1[CH2:7][CH2:8]1)[c:9]1[c:10]([S:11][CH3:12])[n:14][c:15]2[c:16](-[c:17]3[cH:18][cH:19][c:20]([O:21][CH3:22])[cH:23][c:24]3[Cl:25])[n:26][cH:27][cH:28][n:29]12.O=C(O[OH:13])c1cccc(Cl)c1>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH:6]1[CH2:7][CH2:8]1)[c:9]1[c:10]([S:11]([CH3:12])=[O:13]...
CCCN(CC1CC1)c1c(SC)nc2c(-c3ccc(OC)cc3Cl)nccn12.O=C(OO)c1cccc(Cl)c1
CCCN(CC1CC1)c1c(S(C)=O)nc2c(-c3ccc(OC)cc3Cl)nccn12
null
null
ClCCl
Oxidation
Sulfanyl to sulfinyl_peroxide
95b5106b07a173d8eafc1c9c8a6c938befe131c3d1caaf5886529b7aee55ea9d
7652b53bb02130dccfe4b1e8905d7f3db7f05ff3a95a0003c1bab09b1ad4083e
c1ccc(-c2nccn3c(NCC4CC4)cnc23)cc1
Cl-c1:c:c:c:c(-C(=O)-O-[OH;D1;+0:1]):c:1.[#7:2]-[c:3]1:[#7;a:4]2:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:2:[#7;a:10]:[c:11]:1-[S;H0;D2;+0:12]-[C;D1;H3:13]>>[#7:2]-[c:3]1:[#7;a:4]2:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:2:[#7;a:10]:[c:11]:1-[S;H0;D3;+0:12](-[C;D1;H3:13])=[O;H0;D1;+0:1]
12.2
[{"value": 12.2, "product": "ClC1=C(C=CC(=C1)OC)C=1C=2N(C=CN1)C(=C(N2)S(=O)C)N(CCC)CC2CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
m-chloroperbenzoic acid (148 mg) was added to N-[8-(2-chloro-4-methoxyphenyl)-2-(methylsulfanyl)imidazo[1,2-a]pyrazin-3-yl]-N-cyclopropylmethyl-N-propylamine (166 mg) and dichloromethane (2 mL) at room temperature, and the mixture was stirred for 20 minutes. An aqueous sodium thiosulfate solution and an aqueous sodium ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Peroxide.Monosulfide
Sulfoxide
c1ccccc1
null
C1CC1.c1ccccc1.c1cn2ccnc2cn1
HCl
ClCCl
null
0.333333
CCCN(CC1CC1)c1c(SC)nc2c(-c3ccc(OC)cc3Cl)nccn12.O=C(OO)c1cccc(Cl)c1>ClCCl>CCCN(CC1CC1)c1c(S(C)=O)nc2c(-c3ccc(OC)cc3Cl)nccn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-43306c01351343a7af7f36e0fbd02133
CCCN(CC1CC1)c1c(S(C)(=O)=O)nc2c(-c3ccc(OC)cc3Cl)nccn12.C[O-]>>CCCN(CC1CC1)c1c(OC)nc2c(-c3ccc(OC)cc3Cl)nccn12
C[O-].[Na+].ClC1=C(C=CC(=C1)OC)C=1C=2N(C=CN1)C(=C(N2)S(=O)(=O)C)N(CCC)CC2CC2>>ClC1=C(C=CC(=C1)OC)C=1C=2N(C=CN1)C(=C(N2)OC)N(CCC)CC2CC2
CS(=O)(=O)[c:10]1[c:9]([N:4]([CH2:3][CH2:2][CH3:1])[CH2:5][CH:6]2[CH2:7][CH2:8]2)[n:28]2[c:14]([n:13]1)[c:15](-[c:16]1[cH:17][cH:18][c:19]([O:20][CH3:21])[cH:22][c:23]1[Cl:24])[n:25][cH:26][cH:27]2.[O-:11][CH3:12]>>[CH3:1][CH2:2][CH2:3][N:4]([CH2:5][CH:6]1[CH2:7][CH2:8]1)[c:9]1[c:10]([O:11][CH3:12])[n:13][c:14]2[c:15](...
CCCN(CC1CC1)c1c(S(C)(=O)=O)nc2c(-c3ccc(OC)cc3Cl)nccn12.C[O-]
CCCN(CC1CC1)c1c(OC)nc2c(-c3ccc(OC)cc3Cl)nccn12
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
b148c0e9c922e188ff12e3775bf2ce2f392116d80327cd58245aaf623e92a8db
731c19b65b5c8b40ca2c449bc317006921ded977380fbf4f8e42c4e97b0a736b
c1ccc(-c2nccn3c(NCC4CC4)cnc23)cc1
C-S(=O)(=O)-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]2:[c:4]:[#7;a:5]:[c:6]:[c:7]:[#7;a:8]:2:[c:9]:1-[#7:10].[C;D1;H3:11]-[O-;H0;D1:12]>>[#7:10]-[c:9]1:[#7;a:8]2:[c:7]:[c:6]:[#7;a:5]:[c:4]:[c:3]:2:[#7;a:2]:[c;H0;D3;+0:1]:1-[O;H0;D2;+0:12]-[C;D1;H3:11]
null
[]
null
null
6
HOUR
A 28% sodium methoxide solution (5 mL) was added to N[8-(2-chloro-4-methoxyphenyl)-2-(methylsulfonyl)imidazo[1,2-a]pyrazin-3-yl]-N-cyclopropylmethyl-N-propylamine (80 mg), and the mixture was stirred for 6 hours by heating under ref lux. After cooled to room temperature, water was added thereto, which was extracted wit...
10.6084/m9.figshare.5104873.v1
null
Sulfone
Ether
c1cn2ccnc2cn1
c1cn2ccnc2cn1
C1CC1.c1ccccc1.c1cn2ccnc2cn1
HO-
O
null
6
CCCN(CC1CC1)c1c(S(C)(=O)=O)nc2c(-c3ccc(OC)cc3Cl)nccn12.C[O-]>O>CCCN(CC1CC1)c1c(OC)nc2c(-c3ccc(OC)cc3Cl)nccn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8705baba14974396902114f7aa4c7592
COc1ccc(-c2ccnn3c(C(=O)O)c(SC)nc23)c(C)c1.[N-]=[N+]=NP(=O)(c1ccccc1)c1ccccc1>>COc1ccc(-c2ccnn3c(N)c(SC)nc23)c(C)c1
COC1=CC(=C(C=C1)C=1C=2N(N=CC1)C(=C(N2)SC)C(=O)O)C.C(C)(C)(C)O.C(C)N(CC)CC.C1(=CC=CC=C1)P(=O)(C1=CC=CC=C1)N=[N+]=[N-]>>COC1=CC(=C(C=C1)C=1C=2N(N=CC1)C(=C(N2)SC)N)C
O=C(O)[c:12]1[n:11]2[n:10][cH:9][cH:8][c:7](-[c:6]3[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:21][c:19]3[CH3:20])[c:18]2[n:17][c:14]1[S:15][CH3:16].[N-]=[N+]=[N:13]P(=O)(c1ccccc1)c1ccccc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][cH:9][n:10][n:11]3[c:12]([NH2:13])[c:14]([S:15][CH3:16])[n:17][c:18]23)[c:19]([CH3:20])[c...
COc1ccc(-c2ccnn3c(C(=O)O)c(SC)nc23)c(C)c1.[N-]=[N+]=NP(=O)(c1ccccc1)c1ccccc1
COc1ccc(-c2ccnn3c(N)c(SC)nc23)c(C)c1
null
null
O.C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
00fed900d6bd21ee71533bf1e36cf69742e05e0a6a646fdb0a4dd1b86bd1391b
c4869b2e15981984090372c3f8725c0a3f1a2d8cd3a4eec59edd04a0d3b2a386
c1ccc(-c2ccnn3ccnc23)cc1
O-C(=O)-[c;H0;D3;+0:1]1:[#7;a:2](:[#7;a:3]:[c:4]):[c:5]:[#7;a:6]:[c:7]:1-[#16:8].O=P(-[N;H0;D2;+0:9]=[N+]=[N-])(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1>>[#16:8]-[c:7]1:[#7;a:6]:[c:5]:[#7;a:2](:[#7;a:3]:[c:4]):[c;H0;D3;+0:1]:1-[NH2;D1;+0:9]
null
[]
100
CELSIUS
3
HOUR
The resulting 8-(4-methoxy-2-methylphenyl)-2-(methylsulfanyl)imidazo[1,2-b]pyridazine-3-carboxylic acid was dissolved in toluene (10 mL), then tert-butyl alcohol (10 mL), triethylamine (0.49 mL) and diphenylphosphorylazide (0.38 mL) were added thereto, and the mixture was heated at 100° C. for 4 hours. After completion...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Azide
Primary amine
c1cnn2ccnc2c1.c1ccccc1.c1ccccc1
c1cnn2ccnc2c1
c1ccccc1.c1cnn2ccnc2c1
HO-
O.C1(=CC=CC=C1)C
100
3
COc1ccc(-c2ccnn3c(C(=O)O)c(SC)nc23)c(C)c1.[N-]=[N+]=NP(=O)(c1ccccc1)c1ccccc1>O.C1(=CC=CC=C1)C>COc1ccc(-c2ccnn3c(N)c(SC)nc23)c(C)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1b1c1eafe5ed40898117539f0993ce40
CSc1nc2c(Br)cccn2c1CO>>CSc1nc2c(Br)cccn2c1C
BrC=1C=2N(C=CC1)C(=C(N2)SC)CO>>BrC=1C=2N(C=CC1)C(=C(N2)SC)C
O[CH2:13][c:12]1[c:3]([S:2][CH3:1])[n:4][c:5]2[c:6]([Br:7])[cH:8][cH:9][cH:10][n:11]21>>[CH3:1][S:2][c:3]1[n:4][c:5]2[c:6]([Br:7])[cH:8][cH:9][cH:10][n:11]2[c:12]1[CH3:13]
CSc1nc2c(Br)cccn2c1CO
CSc1nc2c(Br)cccn2c1C
null
[O-2].[Mn+4].[O-2]
CC(=O)C
Reduction
OtherReaction
1deafbccd34c1d747dea179c0b63e48cd7fc76936d377fecabe099ecef578991
0a2c8330040d049ae67653e1474aff520bf8a2d8c908ffd7076f536576936945
c1ccn2ccnc2c1
O-[CH2;D2;+0:1]-[c:2]1:[#7;a:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]:1-[#16:8]>>[#16:8]-[c:7]1:[#7;a:6]:[c:5]:[#7;a:3](:[c:4]):[c:2]:1-[CH3;D1;+0:1]
19.9
[{"value": 19.9, "product": "BrC=1C=2N(C=CC1)C(=C(N2)SC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
The resulting [8-bromo-2-(methylsulfanyl)imidazo[1,2-a]pyridin-3-yl]methanol (640 mg) was dissolved in acetone (50 mL), then activated manganese (IV) oxide (4 g) was added thereto, and the mixture was stirred overnight. Manganese (IV) oxide was filtered off through Celite, and the filtrate was evaporated. The resulting...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
null
null
null
c1ccn2ccnc2c1
Other
[O-2].[Mn+4].[O-2].CC(=O)C
null
8
CSc1nc2c(Br)cccn2c1CO>[O-2].[Mn+4].[O-2].CC(=O)C>CSc1nc2c(Br)cccn2c1C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b5311dc1ba214541b9ac95bbd592e777
Cc1ccccc1>>Cc1ccccc1
C1(=CC=CC=C1)C.C1(=CC=CC=C1)C.CS(=O)C.[C@@H]1([C@H](O)[C@H](O)[C@@H](CO)O1)N1C(=O)N=C(N)N=C1.[C@@H]1([C@H](O)[C@H](O)[C@@H](CO)O1)N1C(=O)N=C(N)N=C1.CS(=O)C>>CS(=O)C.C1(=CC=CC=C1)C
[CH3:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1>>[CH3:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1
Cc1ccccc1
Cc1ccccc1
null
null
null
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccccc1
null
null
[]
null
null
null
null
Dimethyl sulfoxide (DMSO) was used as the primary solvent to solubilize Form I of 5-azacytidine and toluene was used as the co-solvent as follows. Approximately 250 mg of 5-azacytidine was dissolved with approximately 5 mL of DMSO, preheated to approximately 90° C., in separate 100-mL beakers. The solids were allowed t...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1
null
null
null
null
Cc1ccccc1>>Cc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-eb7ccf59255147c7a30549f2cc940748
FC(F)=C(F)CCBr.N#C[S-]>>N#CSCCC(F)=C(F)F
BrCCC(=C(F)F)F.[S-]C#N.[NH4+]>>FC(CCSC#N)=C(F)F
Br[CH2:4][CH2:5][C:6]([F:7])=[C:8]([F:9])[F:10].[N:1]#[C:2][S-:3]>>[N:1]#[C:2][S:3][CH2:4][CH2:5][C:6]([F:7])=[C:8]([F:9])[F:10]
FC(F)=C(F)CCBr.N#C[S-]
N#CSCCC(F)=C(F)F
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
4f905981579db6f2866cc0ae1b975a1e274bbb1d618959665eb6b8e4dd6684b9
e26f642c2dc9d150597dcc73347fb476ddd5d717501944aafd09c0558413a369
null
Br-[CH2;D2;+0:1]-[C:2]-[C:3](-[F;D1;H0:4])=[C:5](-[F;D1;H0:6])-[F;D1;H0:7].[N;D1;H0:8]#[C:9]-[S-;H0;D1:10]>>[F;D1;H0:6]-[C:5](-[F;D1;H0:7])=[C:3](-[F;D1;H0:4])-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:10]-[C:9]#[N;D1;H0:8]
null
[]
null
null
null
null
When, for example, 4-bromo-1,1,2-trifluoro-1-butene and ammonium thiocyanate are used, 3,4,4-trifluoro-3-butenyl thiocyanate is obtained which is then reacted with H2S to give 3,4,4-trifluoro-3-butenyl dithiocarbamate. Further reaction of 3,4,4-trifluoro-3-butenyl dithiocarbamate with chloroacetaldehyde then provides 2...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Monosulfide
null
null
null
Br-
null
null
null
FC(F)=C(F)CCBr.N#C[S-]>>N#CSCCC(F)=C(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-56c0a4b08e76451d8ee60e988ae8266a
FC(F)=C(F)CCBr.NC(=S)[S-]>>NC(=S)SCCC(F)=C(F)F
C(N)([S-])=S.[NH4+].BrCCC(=C(F)F)F.C(N)([S-])=S.[NH4+]>>C(N)(SCCC(=C(F)F)F)=S
Br[CH2:5][CH2:6][C:7]([F:8])=[C:9]([F:10])[F:11].[NH2:1][C:2](=[S:3])[S-:4]>>[NH2:1][C:2](=[S:3])[S:4][CH2:5][CH2:6][C:7]([F:8])=[C:9]([F:10])[F:11]
FC(F)=C(F)CCBr.NC(=S)[S-]
NC(=S)SCCC(F)=C(F)F
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
4f905981579db6f2866cc0ae1b975a1e274bbb1d618959665eb6b8e4dd6684b9
e26f642c2dc9d150597dcc73347fb476ddd5d717501944aafd09c0558413a369
null
Br-[CH2;D2;+0:1]-[C:2]-[C:3](-[F;D1;H0:4])=[C:5](-[F;D1;H0:6])-[F;D1;H0:7].[N;D1;H2:8]-[C:9](-[S-;H0;D1:10])=[S;D1;H0:11]>>[F;D1;H0:6]-[C:5](-[F;D1;H0:7])=[C:3](-[F;D1;H0:4])-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:10]-[C:9](-[N;D1;H2:8])=[S;D1;H0:11]
null
[]
40
CELSIUS
3
HOUR
2.8 g (25 mmol) of ammonium dithiocarbamate in 40 ml of ethanol are admixed dropwise with 5.32 g (26.3 mmol; purity 93.2%) of 4-bromo-1,1,2-trifluoro-1-butene, stirred at 40° C. for 3 h, another 2.8 g of ammonium dithiocarbamate is added after 1 h, and everything is left to stand at room temperature for 8 h. The filtra...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Monosulfide
null
null
null
Br-
C(C)O
40
3
FC(F)=C(F)CCBr.NC(=S)[S-]>C(C)O>NC(=S)SCCC(F)=C(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2ce8de5ebde34b87b4c5c63a99ff1610
NC(=S)SCCC(F)=C(F)F>>FC(F)=C(F)CCSc1nccs1
ClCC=O.C(N)(SCCC(=C(F)F)F)=S.Cl.ClCC=O>>FC(CCSC=1SC=CN1)=C(F)F
[F:1][C:2]([F:3])=[C:4]([F:5])[CH2:6][CH2:7][S:8][C:9]([NH2:10])=[S:13]>>[F:1][C:2]([F:3])=[C:4]([F:5])[CH2:6][CH2:7][S:8][c:9]1[n:10][cH:11][cH:12][s:13]1
NC(=S)SCCC(F)=C(F)F
FC(F)=C(F)CCSc1nccs1
null
null
O1CCOCC1
Aromatic Heterocycle Formation
OtherReaction
3c75df89637ec99f54296354329f942342c89ae536c3288455dc37b1a7da8616
c794985a515ce5755267f6637fcb87d41d311c11ef63b51f9b87e88d10f3069c
c1cscn1
[C:1]-[#16:2]-[C;H0;D3;+0:3](-[NH2;D1;+0:4])=[S;H0;D1;+0:5]>>[C:1]-[#16:2]-[c;H0;D3;+0:3]1:[n;H0;D2;+0:4]:[c:6]:[c:7]:[s;H0;D2;+0:5]:1
null
[]
null
null
4
HOUR
15.1 g (64.8 mmol; purity 86.3%) of 3,4,4-trifluoro-3-butenyl dithiocarbamate in 100 ml of dioxane are admixed with 0.2 ml of conc. hydrochloric acid and 12.4 g (71.2 mmol) of 45% aqueous chloroacetaldehyde solution. The mixture is boiled for 4 h under argon, and another 1 ml of chloroacetaldehyde solution is added aft...
10.6084/m9.figshare.5104873.v1
null
Thioamide
Monosulfide
null
c1cscn1
c1cscn1
Other
O1CCOCC1
null
4
NC(=S)SCCC(F)=C(F)F>O1CCOCC1>FC(F)=C(F)CCSc1nccs1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ee4b179577564cf2a3db73ccda4e6fac
CCOC(CCl)OCC.NC(=S)SCCC(F)=C(F)F>>FC(F)=C(F)CCSc1nccs1
C(N)(SCCC(=C(F)F)F)=S.C(C)OC(CCl)OCC.O.C1(=CC=C(C=C1)S(=O)(=O)O)C>>FC(CCSC=1SC=CN1)=C(F)F
CCO[CH:11](OCC)[CH2:12]Cl.[F:1][C:2]([F:3])=[C:4]([F:5])[CH2:6][CH2:7][S:8][C:9]([NH2:10])=[S:13]>>[F:1][C:2]([F:3])=[C:4]([F:5])[CH2:6][CH2:7][S:8][c:9]1[n:10][cH:11][cH:12][s:13]1
CCOC(CCl)OCC.NC(=S)SCCC(F)=C(F)F
FC(F)=C(F)CCSc1nccs1
null
null
C(C)(=O)O
Aromatic Heterocycle Formation
OtherReaction
99b4763ff7b16f88720d53459ef736995aaa64d13ca13967d7f53851cba3e9f7
42d1ee8bd24936aec7c7b6a0e0cb3c7e317f16436defca54664117f832e663aa
c1cscn1
C-C-O-[CH;D3;+0:1](-O-C-C)-[CH2;D2;+0:2]-Cl.[C:3]-[#16:4]-[C;H0;D3;+0:5](-[NH2;D1;+0:6])=[S;H0;D1;+0:7]>>[C:3]-[#16:4]-[c;H0;D3;+0:5]1:[n;H0;D2;+0:6]:[cH;D2;+0:1]:[cH;D2;+0:2]:[s;H0;D2;+0:7]:1
null
[]
95
CELSIUS
1.5
HOUR
3 g (14.9 mmol) of 3,4,4-trifluoro-3-butenyl dithiocarbamate in 15 ml of glacial acetic acid are admixed with 2.3 g (15.1 mmol) of chloroacetaldehyde diethyl acetal and 40 mg of p-toluenesulphonic acid monohydrate. The mixture is stirred at 95° C. for 1.5 h and, after cooling to room temperature, is then concentrated b...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Thioamide.Monosulfide
Monosulfide
null
c1cscn1
c1cscn1
HCl
C(C)(=O)O
95
1.5
CCOC(CCl)OCC.NC(=S)SCCC(F)=C(F)F>C(C)(=O)O>FC(F)=C(F)CCSc1nccs1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0e5e586dc80948d58ac7c0774a324757
COc1ccc(CNc2nc(N3CCC[C@H]3CO)ncc2C=O)cc1Cl>>C=C[C@H](CO)c1cnc(N2CCCC2CO)nc1NCc1ccc(OC)c(Cl)c1
OC[C@H]1N(CCC1)C1=NC=C(C(=N1)NCC1=CC(=C(C=C1)OC)Cl)C=O.C(=C)[Mg]Br.O1CCCC1.O1CCCC1.[Cl-].[NH4+]>>OCC1N(CCC1)C1=NC=C(C(=N1)NCC1=CC(=C(C=C1)OC)Cl)[C@H](C=C)CO
[CH:3](=[O:5])[c:6]1[cH:7][n:8][c:9]([N:10]2[CH2:11][CH2:12][CH2:13][C@H:14]2[CH2:15][OH:16])[n:17][c:18]1[NH:19][CH2:20][c:21]1[cH:22][cH:23][c:24]([O:25][CH3:26])[c:27]([Cl:28])[cH:29]1>>[CH2:1]=[CH:2][C@H:3]([CH2:4][OH:5])[c:6]1[cH:7][n:8][c:9]([N:10]2[CH2:11][CH2:12][CH2:13][CH:14]2[CH2:15][OH:16])[n:17][c:18]1[NH:...
COc1ccc(CNc2nc(N3CCC[C@H]3CO)ncc2C=O)cc1Cl
C=C[C@H](CO)c1cnc(N2CCCC2CO)nc1NCc1ccc(OC)c(Cl)c1
null
null
null
Miscellaneous
OtherReaction
155e7013e16dbd44eda1307fb1d28f7a05e58bf69dec69e6af17a470120ea006
2e5da6f4774f1c79021a74214574517f5452fdf09afdcef5a464ff4f1128a852
c1ccc(CNc2ccnc(N3CCCC3)n2)cc1
[#7:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1-[CH;D2;+0:8]=[O;H0;D1;+0:9]>>[#7:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1-[C@H;D3;+0:8](-[C:10]=[C;D1;H2:11])-[C:12]-[OH;D1;+0:9]
null
[]
0
CELSIUS
1
HOUR
A solution of (S)-2-(2-hydroxymethyl-1-pyrrolidinyl)-5-formyl-4-(3-chloro-4-methoxybenzylamino)pyrimidine (4.1 g) in tetrahydrofuran (30 ml) is added to a solution of vinyl magnesium bromide in tetrahydrofuran (43.5 ml) at 0° C., and the mixture is stirred at 0° C. for 1 hour. To the mixture is added a saturated aqueou...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Primary alcohol.Vinyl
null
null
c1cncnc1.C1CC[NH]C1.c1ccccc1
Other
null
0
1
COc1ccc(CNc2nc(N3CCC[C@H]3CO)ncc2C=O)cc1Cl>>C=C[C@H](CO)c1cnc(N2CCCC2CO)nc1NCc1ccc(OC)c(Cl)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e5f8271f05a748aca5b142ffca477532
CCCc1[nH]cnc1C(=O)OCC>>CCCc1[nH]cnc1C(=O)O
C(C)OC(=O)C=1N=CNC1CCC.Cl>>Cl.C(CC)C1=C(N=CN1)C(=O)O
CC[O:11][C:9]([c:8]1[c:4]([CH2:3][CH2:2][CH3:1])[nH:5][cH:6][n:7]1)=[O:10]>>[CH3:1][CH2:2][CH2:3][c:4]1[nH:5][cH:6][n:7][c:8]1[C:9](=[O:10])[OH:11]
CCCc1[nH]cnc1C(=O)OCC
CCCc1[nH]cnc1C(=O)O
null
null
O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1c[nH]cn1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4](:[#7;a:5]):[c:6]:[#7;a:7]>>[#7;a:7]:[c:6]:[c:4](-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]):[#7;a:5]
100
[{"value": 100.0, "product": "Cl.C(CC)C1=C(N=CN1)C(=O)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
5-Propyl-1H-imidazole-4-carboxylic acid ethyl ester 2 (2.00 g; 11.0 mmol) and concentrated aqueous HCl (40 mL) were combined and heated to reflux with stirring for 24 h. After cooling to rt, the light tan solution was diluted with water (100 mL) and extracted with EtOAc. The aqueous layer was then evaporated under redu...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1c[nH]cn1
Other
O
null
24
CCCc1[nH]cnc1C(=O)OCC>O>CCCc1[nH]cnc1C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dc241ef9e78942adaf22ff1337bff403
CCCc1[nH]cnc1C(=O)O.O=C(Cl)C(=O)Cl>>CCCc1[nH]cnc1C(=O)Cl
Cl.C(CC)C1=C(N=CN1)C(=O)O.C(C(=O)Cl)(=O)Cl>>C(CC)C1=C(N=CN1)C(=O)Cl
O[C:9]([c:8]1[c:4]([CH2:3][CH2:2][CH3:1])[nH:5][cH:6][n:7]1)=[O:10].O=C(Cl)C(=O)[Cl:11]>>[CH3:1][CH2:2][CH2:3][c:4]1[nH:5][cH:6][n:7][c:8]1[C:9](=[O:10])[Cl:11]
CCCc1[nH]cnc1C(=O)O.O=C(Cl)C(=O)Cl
CCCc1[nH]cnc1C(=O)Cl
null
null
null
Functional Group Interconversion
Alcohol to chloride_Other
013cec2edeb273a7a148f349d36a52d99ff4e7bcf8eed78085df830088e387ac
aedb1f68dc5b7eb0583043e1125b741382b17974140a2f46554f0110e2ddc884
c1c[nH]cn1
Cl-C(=O)-C(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[c:4]1:[#7;a:5]:[c:6]:[#7;a:7]:[c:8]:1-[C:9]>>[C:9]-[c:8]1:[#7;a:7]:[c:6]:[#7;a:5]:[c:4]:1-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3]
71.1
[{"value": 71.0, "product": "C(CC)C1=C(N=CN1)C(=O)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 71.1, "product": "C(CC)C1=C(N=CN1)C(=O)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
5-Propyl-1H-imidazole-4-carboxylic acid hydrochloride 3 (1.0 g; 5.3 mmol) was added to nitrogen-purged CH3CN (10 mL). Oxalyl chloride (2.5 ml; 29 mmol) was then added, and the mixture was heated to reflux under N2 for 1 h. The brown solution was then allowed to cool, and the product began to precipitate. Ice-cold dry E...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Carboxylic acid
Acyl halide
null
null
c1c[nH]cn1
HCl
null
null
null
CCCc1[nH]cnc1C(=O)O.O=C(Cl)C(=O)Cl>>CCCc1[nH]cnc1C(=O)Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c5c47ba74d2c4e2f8477997e73d47b11
CCCc1[nH]c(I)nc1C(=O)NC>>CCCc1[nH]c(-c2nc(C(=O)NC)c(CCC)[nH]2)nc1C(=O)NC
CNC(=O)C=1N=C(NC1CCC)I>>CNC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NC)CCC
I[c:6]1[nH:5][c:4]([CH2:3][CH2:2][CH3:1])[c:20]([C:10](=[O:11])[NH:12][CH3:13])[n:8]1>>[CH3:1][CH2:2][CH2:3][c:4]1[nH:5][c:6](-[c:7]2[n:8][c:9]([C:10](=[O:11])[NH:12][CH3:13])[c:14]([CH2:15][CH2:16][CH3:17])[nH:18]2)[n:19][c:20]1[C:21](=[O:22])[NH:23][CH3:24]
CCCc1[nH]c(I)nc1C(=O)NC
CCCc1[nH]c(-c2nc(C(=O)NC)c(CCC)[nH]2)nc1C(=O)NC
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
cf1d90069438d2f20a6c3db28aa27e3ffc2ce5318cd39d02979dd772a5545e51
75ef3d1db8ed5627cad9f1c04eeb05e1be73f58c43a4d9b45880972cbc9d3ec3
c1c[nH]c(-c2ncc[nH]2)n1
I-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[C:4]):[c;H0;D3;+0:5](-[C;H0;D3;+0:6](=[O;D1;H0:7])-[#7:8]-[C;D1;H3:9]):[n;H0;D2;+0:10]:1>>[#7:11]-[C:12](=[O;D1;H0:13])-[c;H0;D3;+0:5]1:[#7;a:14]:[c;H0;D3;+0:1](-[c:15]2:[#7;a:16]:[c:17]:[c:18](-[C;H0;D3;+0:6](=[O;D1;H0:7])-[#7:8]-[C;D1;H3:9]):[n;H0;D2;+0:10]:2):[#7;a:2]:[c:3]:1-[C:4]
43
[{"value": 43.0, "product": "CNC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NC)CCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 40.1, "product": "CNC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Iodide 6a (0.35 g; 1.2 mmol) was used as starting material. After cooling to rt, the reaction mixture was diluted with CH3OH and filtered. The filtrate was evaporated under vacuum, and the residue was dissolved in CH2Cl2. Upon standing, a white solid precipitated. This material was collected by filtration and was washe...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amide
Secondary amide.Secondary amide
c1c[nH]cn1
c1c[nH]cn1.c1c[nH]cn1
c1c[nH]cn1.c1c[nH]cn1
I-
CO
null
null
CCCc1[nH]c(I)nc1C(=O)NC>CO>CCCc1[nH]c(-c2nc(C(=O)NC)c(CCC)[nH]2)nc1C(=O)NC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0530478446b848d8948fd58216e836f3
CCCc1[nH]c(I)nc1C(=O)NCc1cc(F)cc(F)c1>>CCCc1[nH]c(-c2nc(C(=O)NCc3cc(F)cc(F)c3)c(CCC)[nH]2)nc1C(=O)NCc1cc(F)cc(F)c1
FC=1C=C(CNC(=O)C=2N=C(NC2CCC)I)C=C(C1)F>>FC=1C=C(CNC(=O)C=2N=C(NC2CCC)C=2NC(=C(N2)C(=O)NCC2=CC(=CC(=C2)F)F)CCC)C=C(C1)F
I[c:7]1[nH:5][c:4]([CH2:3][CH2:2][CH3:1])[c:28]([C:10](=[O:11])[NH:12][CH2:13][c:14]2[cH:6][c:33]([F:17])[cH:18][c:19]([F:20])[cH:21]2)[n:8]1>>[CH3:1][CH2:2][CH2:3][c:4]1[nH:5][c:6](-[c:7]2[n:8][c:9]([C:10](=[O:11])[NH:12][CH2:13][c:14]3[cH:15][c:16]([F:17])[cH:18][c:19]([F:20])[cH:21]3)[c:22]([CH2:23][CH2:24][CH3:25])...
CCCc1[nH]c(I)nc1C(=O)NCc1cc(F)cc(F)c1
CCCc1[nH]c(-c2nc(C(=O)NCc3cc(F)cc(F)c3)c(CCC)[nH]2)nc1C(=O)NCc1cc(F)cc(F)c1
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
cff40fbdd314028511f4604655acaaf7b0df6b4cf2cd2bce957aa6cbea338c87
28393239e30c0319b195347defa439702c27770d21b5c3de4f0075a7ffe10e1d
O=C(NCc1ccccc1)c1c[nH]c(-c2nc(C(=O)NCc3ccccc3)c[nH]2)n1
I-[c;H0;D3;+0:1]1:[n;H0;D2;+0:2]:[c;H0;D3;+0:3](-[C;H0;D3;+0:4](=[O;D1;H0:5])-[#7:6]-[C:7]-[c;H0;D3;+0:8]2:[c:9]:[c:10](-[F;D1;H0:11]):[cH;D2;+0:12]:[c;H0;D3;+0:13](-[F;H0;D1;+0:14]):[cH;D2;+0:15]:2):[c:16](-[C:17]):[nH;D2;+0:18]:1>>[C:17]-[c:16]1:[nH;D2;+0:18]:[c;H0;D3;+0:15](-[c;H0;D3;+0:1]2:[#7;a:19]:[c:20]:[c:21](-...
40
[{"value": 40.0, "product": "FC=1C=C(CNC(=O)C=2N=C(NC2CCC)C=2NC(=C(N2)C(=O)NCC2=CC(=CC(=C2)F)F)CCC)C=C(C1)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 39.2, "product": "FC=1C=C(CNC(=O)C=2N=C(NC2CCC)C=2NC(=C(N2)C(=O)NCC2=CC(=CC(=C2)F)F)CCC)C=C(C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": f...
null
null
null
null
Iodide 6b (0.44 g; 1.1 mmol) was used as starting material. After cooling to rt, the reaction mixture was diluted with CH3OH and filtered. The filtrate was evaporated under vacuum, and the residue was dissolved in CHCl3. Slow addition of CH3CN caused a brown solid to precipitate. This material was collected by filtrati...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Secondary amide
Aromatic halide.Aromatic halide.Aromatic halide.Secondary amide.Secondary amide
c1c[nH]cn1.c1ccccc1
c1c[nH]cn1.c1c[nH]cn1.c1ccccc1.c1ccccc1
c1c[nH]cn1.c1c[nH]cn1.c1ccccc1.c1ccccc1
I-
CO
null
null
CCCc1[nH]c(I)nc1C(=O)NCc1cc(F)cc(F)c1>CO>CCCc1[nH]c(-c2nc(C(=O)NCc3cc(F)cc(F)c3)c(CCC)[nH]2)nc1C(=O)NCc1cc(F)cc(F)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3c49c3434b894b6baf6695c4233a0826
CCCc1[nH]c(I)nc1C(=O)NCc1ccc(C)cc1>>CCCc1[nH]c(-c2nc(C(=O)NCc3ccc(C)cc3)c(CCC)[nH]2)nc1C(=O)NCc1ccc(C)cc1
CC1=CC=C(CNC(=O)C=2N=C(NC2CCC)I)C=C1>>CC1=CC=C(CNC(=O)C=2N=C(NC2CCC)C=2NC(=C(N2)C(=O)NCC2=CC=C(C=C2)C)CCC)C=C1
I[c:7]1[nH:5][c:4]([CH2:3][CH2:2][CH3:1])[c:27]([C:10](=[O:11])[NH:12][CH2:13][c:14]2[cH:6][cH:16][c:17]([CH3:18])[cH:19][cH:20]2)[n:8]1>>[CH3:1][CH2:2][CH2:3][c:4]1[nH:5][c:6](-[c:7]2[n:8][c:9]([C:10](=[O:11])[NH:12][CH2:13][c:14]3[cH:15][cH:16][c:17]([CH3:18])[cH:19][cH:20]3)[c:21]([CH2:22][CH2:23][CH3:24])[nH:25]2)[...
CCCc1[nH]c(I)nc1C(=O)NCc1ccc(C)cc1
CCCc1[nH]c(-c2nc(C(=O)NCc3ccc(C)cc3)c(CCC)[nH]2)nc1C(=O)NCc1ccc(C)cc1
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
cd8f9849305f10187a62b17e80cb088e7ea2eb0c51b2f0b25cbf9ed71b37c27b
75ef3d1db8ed5627cad9f1c04eeb05e1be73f58c43a4d9b45880972cbc9d3ec3
O=C(NCc1ccccc1)c1c[nH]c(-c2nc(C(=O)NCc3ccccc3)c[nH]2)n1
I-[c;H0;D3;+0:1]1:[n;H0;D2;+0:2]:[c;H0;D3;+0:3](-[C;H0;D3;+0:4](=[O;D1;H0:5])-[#7:6]-[C:7]-[c;H0;D3;+0:8]2:[c:9]:[c:10]:[c:11](-[C;D1;H3:12]):[cH;D2;+0:13]:[cH;D2;+0:14]:2):[c:15](-[C:16]):[nH;D2;+0:17]:1>>[#7:18]-[C:19](=[O;D1;H0:20])-[c;H0;D3;+0:3]1:[#7;a:21]:[c;H0;D3;+0:14](-[c;H0;D3;+0:1]2:[#7;a:22]:[c:23]:[c:24](-...
97.5
[{"value": 38.0, "product": "CC1=CC=C(CNC(=O)C=2N=C(NC2CCC)C=2NC(=C(N2)C(=O)NCC2=CC=C(C=C2)C)CCC)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.5, "product": "CC1=CC=C(CNC(=O)C=2N=C(NC2CCC)C=2NC(=C(N2)C(=O)NCC2=CC=C(C=C2)C)CCC)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Iodide 6c (0.45 g; 1.2 mmol) was used as starting material. After cooling to rt, the reaction mixture was diluted with CH3OH and filtered. The filtrate was evaporated under vacuum, and the residue was triturated with CH3CN. The solid that remained undissolved was collected by filtration and washed with CH3CN to afford ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amide
Secondary amide.Secondary amide
c1c[nH]cn1.c1ccccc1
c1c[nH]cn1.c1c[nH]cn1.c1ccccc1.c1ccccc1
c1c[nH]cn1.c1c[nH]cn1.c1ccccc1.c1ccccc1
I-
CO
null
null
CCCc1[nH]c(I)nc1C(=O)NCc1ccc(C)cc1>CO>CCCc1[nH]c(-c2nc(C(=O)NCc3ccc(C)cc3)c(CCC)[nH]2)nc1C(=O)NCc1ccc(C)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d2419e508c674da0968fc6df07f52955
CCCCCCNC(=O)c1nc(I)[nH]c1CCC>>CCCCCCNC(=O)c1nc(-c2nc(C(=O)NCCCCCC)c(CCC)[nH]2)[nH]c1CCC
C(CCCCC)NC(=O)C=1N=C(NC1CCC)I>>C(CCCCC)NC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NCCCCCC)CCC
I[c:12]1[n:7][c:10]([C:8](=[O:9])[NH:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:1])[c:31]([CH2:32][CH2:33][CH3:34])[nH:30]1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][NH:7][C:8](=[O:9])[c:10]1[n:11][c:12](-[c:13]2[n:14][c:15]([C:16](=[O:17])[NH:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[c:25]([CH2:26][C...
CCCCCCNC(=O)c1nc(I)[nH]c1CCC
CCCCCCNC(=O)c1nc(-c2nc(C(=O)NCCCCCC)c(CCC)[nH]2)[nH]c1CCC
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
cf1d90069438d2f20a6c3db28aa27e3ffc2ce5318cd39d02979dd772a5545e51
75ef3d1db8ed5627cad9f1c04eeb05e1be73f58c43a4d9b45880972cbc9d3ec3
c1c[nH]c(-c2ncc[nH]2)n1
I-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[C:4]):[c;H0;D3;+0:5](-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:8]-[C:9]-[C:10]-[C:11]-[C:12]-[CH2;D2;+0:13]-[CH3;D1;+0:14]):[n;H0;D2;+0:15]:1>>[#7;a:16]:[c:17](-[c;H0;D3;+0:1]1:[#7;a:18]:[c;H0;D3;+0:5](-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:15]-[C:19]-[C:20]):[c:3](-[C:4]):[#7;a:2]:1):...
46.2
[{"value": 45.0, "product": "C(CCCCC)NC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NCCCCCC)CCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 46.2, "product": "C(CCCCC)NC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NCCCCCC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Iodide 6d (0.45 g; 1.1 mmol) was used as starting material. After cooling to rt, the reaction mixture was diluted with CH3OH and filtered. The filtrate was evaporated under vacuum, and the residue was recrystallized from CH3OH to afford 0.12 g (45%) of 1d as a white solid. mp>260 C; TLC (CH2Cl2-EtOAc, 1:1): Rf=0.51; 1H...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amide
Secondary amide.Secondary amide
c1c[nH]cn1
c1c[nH]cn1.c1c[nH]cn1
c1c[nH]cn1.c1c[nH]cn1
I-
CO
null
null
CCCCCCNC(=O)c1nc(I)[nH]c1CCC>CO>CCCCCCNC(=O)c1nc(-c2nc(C(=O)NCCCCCC)c(CCC)[nH]2)[nH]c1CCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-caba9355756548b0a75c50b05894c6a7
CCCc1[nH]c(I)nc1C(=O)NCCCOC>>CCCc1[nH]c(-c2nc(C(=O)NCCCOC)c(CCC)[nH]2)nc1C(=O)NCCCOC
COCCCNC(=O)C=1N=C(NC1CCC)I>>COCCCNC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NCCCOC)CCC
I[c:6]1[nH:5][c:4]([CH2:3][CH2:2][CH3:1])[c:24]([C:25](=[O:11])[NH:27][CH2:28][CH2:29][CH2:30][O:31][CH3:32])[n:8]1>>[CH3:1][CH2:2][CH2:3][c:4]1[nH:5][c:6](-[c:7]2[n:8][c:9]([C:10](=[O:11])[NH:12][CH2:13][CH2:14][CH2:15][O:16][CH3:17])[c:18]([CH2:19][CH2:20][CH3:21])[nH:22]2)[n:23][c:24]1[C:25](=[O:26])[NH:27][CH2:28][...
CCCc1[nH]c(I)nc1C(=O)NCCCOC
CCCc1[nH]c(-c2nc(C(=O)NCCCOC)c(CCC)[nH]2)nc1C(=O)NCCCOC
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
26a5c7af5a9622d67ebeeec655718957946a08ae3f1b634d9ccb4d435f86813a
4d88ea68dd05fb8223fde8371077f4656c83c406ef12a864fa6252b2c1c92346
c1c[nH]c(-c2ncc[nH]2)n1
I-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[C:4]):[c;H0;D3;+0:5](-[C;H0;D3;+0:6](=[O;H0;D1;+0:7])-[#7:8]-[C:9]):[n;H0;D2;+0:10]:1>>[#7:11]-[C:12](=[O;H0;D1;+0:7])-[c:13]1:[c:14]:[#7;a:15]:[c:16](-[c;H0;D3;+0:1]2:[#7;a:17]:[c;H0;D3;+0:5](-[C;H0;D3;+0:6](=[O;D1;H0:18])-[#7:8]-[C:9]):[c:3](-[C:4]):[#7;a:2]:2):[n;H0;D2;+0:10]:1
36.2
[{"value": 33.0, "product": "COCCCNC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NCCCOC)CCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 36.2, "product": "COCCCNC(=O)C=1N=C(NC1CCC)C=1NC(=C(N1)C(=O)NCCCOC)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Iodide 6e (0.55 g; 1.6 mmol) was used as starting material. After cooling to rt, the reaction mixture was diluted with CH3OH and filtered. The filtrate was evaporated under vacuum, and the residue was recrystallized from EtOAc to afford 0.13 g (33%) of 1e as colorless prisms. mp>260 C; TLC (EtOAc): Rf=0.31; 1H NMR (CDC...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amide
Ether.Secondary amide.Secondary amide
c1c[nH]cn1
c1c[nH]cn1.c1c[nH]cn1
c1c[nH]cn1.c1c[nH]cn1
I-
CO
null
null
CCCc1[nH]c(I)nc1C(=O)NCCCOC>CO>CCCc1[nH]c(-c2nc(C(=O)NCCCOC)c(CCC)[nH]2)nc1C(=O)NCCCOC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1471d6ffb8994112af60f9816c4686ad
CCCc1[nH]c(I)nc1C(=O)N1CCCC1>>CCCc1[nH]c(-c2nc(C(=O)N3CCCC3)c(CCC)[nH]2)nc1C(=O)N1CCCC1
IC=1NC(=C(N1)C(=O)N1CCCC1)CCC>>C(CC)C1=C(N=C(N1)C=1NC(=C(N1)C(=O)N1CCCC1)CCC)C(=O)N1CCCC1
I[c:6]1[nH:5][c:4]([CH2:3][CH2:2][CH3:1])[c:23]([C:10](=[O:11])[N:12]2[CH2:7][CH2:14][CH2:15][CH2:16]2)[n:8]1>>[CH3:1][CH2:2][CH2:3][c:4]1[nH:5][c:6](-[c:7]2[n:8][c:9]([C:10](=[O:11])[N:12]3[CH2:13][CH2:14][CH2:15][CH2:16]3)[c:17]([CH2:18][CH2:19][CH3:20])[nH:21]2)[n:22][c:23]1[C:24](=[O:25])[N:26]1[CH2:27][CH2:28][CH2...
CCCc1[nH]c(I)nc1C(=O)N1CCCC1
CCCc1[nH]c(-c2nc(C(=O)N3CCCC3)c(CCC)[nH]2)nc1C(=O)N1CCCC1
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
b19d816bdadaa0452545a7bf101eb5b5fec54720ee6b6e7ab221b1b3f69f7e03
03a4c0e057232c9f8ddafedbd062feb799e61aa63113f7c9543c725ec07158be
O=C(c1c[nH]c(-c2nc(C(=O)N3CCCC3)c[nH]2)n1)N1CCCC1
I-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[C:4]):[c;H0;D3;+0:5](-[C;H0;D3;+0:6](=[O;D1;H0:7])-[N;H0;D3;+0:8]2-[C:9]-[C:10]-[CH2;D2;+0:11]-[CH2;D2;+0:12]-2):[n;H0;D2;+0:13]:1>>[#7:14]-[C:15](=[O;D1;H0:16])-[c;H0;D3;+0:5]1:[#7;a:17]:[c;H0;D3;+0:1](-[c;H0;D3;+0:12]2:[#7;a:18]:[c:19]:[c:20](-[C;H0;D3;+0:6](=[O;D1;H0:7])-[N;H0;D3;+...
38.8
[{"value": 38.0, "product": "C(CC)C1=C(N=C(N1)C=1NC(=C(N1)C(=O)N1CCCC1)CCC)C(=O)N1CCCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 38.8, "product": "C(CC)C1=C(N=C(N1)C=1NC(=C(N1)C(=O)N1CCCC1)CCC)C(=O)N1CCCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Iodide 6f (0.34 g; 1.0 mmol) was used as starting material. After cooling to rt, the reaction mixture was diluted with CH3OH and filtered. The filtrate was evaporated under vacuum, and the residue was recrystallized from CH3OH to afford 0.080 g (38%) of 1f as yellow prisms. mp>260 C; TLC (EtOAc): Rf=0.14; 1H NMR (DMSO-...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tertiary amide
Tertiary amide.Tertiary amide
c1c[nH]cn1.C1CC[NH]C1
c1c[nH]cn1.c1c[nH]cn1.C1CC[NH]C1.C1CC[NH]C1
c1c[nH]cn1.c1c[nH]cn1.C1CC[NH]C1.C1CC[NH]C1
I-
CO
null
null
CCCc1[nH]c(I)nc1C(=O)N1CCCC1>CO>CCCc1[nH]c(-c2nc(C(=O)N3CCCC3)c(CCC)[nH]2)nc1C(=O)N1CCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f4e0a65a32994fa48f9d8ab4994782e3
CC(C)(C)OC(=O)NCCOCCO.CS(=O)(=O)Cl>>CC(C)(C)OC(=O)NCCOCCOS(C)(=O)=O
OCCOCCNC(OC(C)(C)C)=O.C(C)N(CC)CC.CS(=O)(=O)Cl>>CS(=O)(=O)OCCOCCNC(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][OH:14].Cl[S:15]([CH3:16])(=[O:17])=[O:18]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][O:14][S:15]([CH3:16])(=[O:17])=[O:18]
CC(C)(C)OC(=O)NCCOCCO.CS(=O)(=O)Cl
CC(C)(C)OC(=O)NCCOCCOS(C)(=O)=O
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
null
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6]-[OH;D1;+0:7]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
97.4
[{"value": 97.4, "product": "CS(=O)(=O)OCCOCCNC(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
22
HOUR
A rapidly stirred solution of tert-butyl 2-(2-hydroxyethoxy)ethylcarbamate (47.1 g, 0.230 mol) in 1 L of anhydrous CH2Cl2 was cooled to 0° C. under N2 and treated with triethylamine (48.0 mL, 0.345 mol). Methanesulfonyl chloride (19.6 mL, 0.253 mol) was then added dropwise over 30 min. The reaction mixture was then all...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
null
HCl
C(Cl)Cl
null
22
CC(C)(C)OC(=O)NCCOCCO.CS(=O)(=O)Cl>C(Cl)Cl>CC(C)(C)OC(=O)NCCOCCOS(C)(=O)=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-38d8fd0ae2e647af882a24d804a170c3
CC(C)(C)OC(=O)NCCOCCOS(C)(=O)=O.[N-]=[N+]=[N-]>>CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-]
O.CS(=O)(=O)OCCOCCNC(=O)OC(C)(C)C.[N-]=[N+]=[N-].[Na+]>>N(=[N+]=[N-])CCOCCNC(OC(C)(C)C)=O
CS(=O)(=O)O[CH2:13][CH2:12][O:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7].[N-:14]=[N+:15]=[N-:16]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][N:14]=[N+:15]=[N-:16]
CC(C)(C)OC(=O)NCCOCCOS(C)(=O)=O.[N-]=[N+]=[N-]
CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-]
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
341eb24906c58cd9cfdeec13febaf0724780d7854e6b6d7ec703218c4bcbe27b
5f2cb2b9819a73a6855f5277f7fe9d5ce3871340baaebb59d42e38e1ca145c0a
null
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[#8:3].[N-;H0;D1:4]=[#7;+:5]=[N;-;D1;H0:6]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D2;+0:4]=[#7;+:5]=[N;-;D1;H0:6]
100.8
[{"value": 100.8, "product": "N(=[N+]=[N-])CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
90
CELSIUS
5
HOUR
A stirred solution of 2-{2-[(tert-butoxycarbonyl)amino]ethoxy}ethyl methanesulfonate (63.5 g, 0.224 mol) in 400 mL of N,N-dimethylformamide (DMF) was treated with NaN3 (16.1 g, 0.247 mol) and the reaction mixture was heated to 90° C. under N2. After 5 h, the solution was cooled to room temperature and treated with 500 ...
10.6084/m9.figshare.5104873.v1
null
Mesylate
Azide
null
null
null
MsOH.HO-
CN(C=O)C
90
5
CC(C)(C)OC(=O)NCCOCCOS(C)(=O)=O.[N-]=[N+]=[N-]>CN(C=O)C>CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-]
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-31b7aba47286438e835babc150ae9da8
CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-]>>CC(C)(C)OC(=O)NCCOCCN
N(=[N+]=[N-])CCOCCNC(OC(C)(C)C)=O>>NCCOCCNC(OC(C)(C)C)=O
[N-]=[N+]=[N:14][CH2:13][CH2:12][O:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH2:14]
CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-]
CC(C)(C)OC(=O)NCCOCCN
null
[Pd]
CO
Reduction
Azide to amine reduction (Staudinger)
4c9e4990dae2bb965dec06bd45e318560989ee3681b61e443f7aa363b7cfa222
cd009d687d606bf351eac9390a176d16be38f2c8216a599b398641009c215027
null
[C:1]-[C:2]-[N;H0;D2;+0:3]=[N+]=[N-]>>[C:1]-[C:2]-[NH2;D1;+0:3]
84.7
[{"value": 84.7, "product": "NCCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution of tert-butyl 2-(2-azidoethoxy)ethylcarbamate (47.0 g, 0.204 mol) in MeOH was treated with 4 g of 10% Pd on carbon and shaken under H2 (3 Kg/cm2) for 24 h. The solution was then filtered through a Celite pad and concentrated to give 35.3 g of crude tert-butyl 2-(2-aminoethoxy)ethylcarbamate as a colorless li...
10.6084/m9.figshare.5104873.v1
null
Azide
Primary amine
null
null
null
Other
[Pd].CO
null
24
CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-]>[Pd].CO>CC(C)(C)OC(=O)NCCOCCN
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-76cccbeb34944a19aefdb50e87f8a8b2
CC(C)(C)OC(=O)NCCOCCN.O=[N+]([O-])c1cnc2ccccc2c1Cl>>CC(C)(C)OC(=O)NCCOCCNc1c([N+](=O)[O-])cnc2ccccc12
ClC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-].C(C)N(CC)CC.NCCOCCNC(OC(C)(C)C)=O>>[N+](=O)([O-])C=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH2:14].Cl[c:15]1[c:16]([N+:17](=[O:18])[O-:19])[cH:20][n:21][c:22]2[cH:23][cH:24][cH:25][cH:26][c:27]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH:14][c:15]1[c:16]([N+:17](=[...
CC(C)(C)OC(=O)NCCOCCN.O=[N+]([O-])c1cnc2ccccc2c1Cl
CC(C)(C)OC(=O)NCCOCCNc1c([N+](=O)[O-])cnc2ccccc12
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2ncccc2c1
Cl-[c;H0;D3;+0:1]1:[c:2](-[#7;+:3]):[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8]:1:[c:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:3]-[c:2]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
76.7
[{"value": 76.7, "product": "[N+](=O)([O-])C=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A stirred solution of 4-chloro-3-nitroquinoline (31.4 g, 0.151 mol) in 500 mL of anhydrous CH2Cl2, under N2, was treated with triethylamine (43 mL, 0.308 mol) and tert-butyl 2-(2-aminoethoxy)ethylcarbamate (0.151 mol). After stirring overnight, the reaction mixture was washed with H2O (2×300 mL) and brine (300 mL). The...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
C(Cl)Cl
null
8
CC(C)(C)OC(=O)NCCOCCN.O=[N+]([O-])c1cnc2ccccc2c1Cl>C(Cl)Cl>CC(C)(C)OC(=O)NCCOCCNc1c([N+](=O)[O-])cnc2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ffc2f0b837a140e68c0db5793f01c784
CC(C)(C)OC(=O)NCCOCCNc1c([N+](=O)[O-])cnc2ccccc12>>CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12
[N+](=O)([O-])C=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O>>NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O
O=[N+:17]([O-])[c:16]1[c:15]([NH:14][CH2:13][CH2:12][O:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[c:25]2[c:20]([n:19][cH:18]1)[cH:21][cH:22][cH:23][cH:24]2>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH:14][c:15]1[c:16]([NH2:17])[cH:18][n:1...
CC(C)(C)OC(=O)NCCOCCNc1c([N+](=O)[O-])cnc2ccccc12
CC(C)(C)OC(=O)NCCOCCNc1c(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]
99.9
[{"value": 99.9, "product": "NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution of tert-butyl 2-{2-[(3-nitroquinolin-4-yl)amino]ethoxy}ethylcarbamate (7.52 g, 20.0 mmol) in toluene was treated with 1.5 g of 5% Pt on carbon and shaken under H2 (3 Kg/cm2) for 24 h. The solution was then filtered through a Celite pad and concentrated to give 6.92 g of crude tert-butyl 2-{2-[(3-aminoquinoli...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C1(=CC=CC=C1)C
null
24
CC(C)(C)OC(=O)NCCOCCNc1c([N+](=O)[O-])cnc2ccccc12>[Pt].C1(=CC=CC=C1)C>CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9efc1cb544b0485cad9fea828694f51d
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.COCCC(=O)Cl>>COCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
C.COCCC(=O)Cl.C(C)N(CC)CC.NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O.C(C)N(CC)CC>>COCCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O
[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1[NH:17][CH2:18][CH2:19][O:20][CH2:21][CH2:22][NH:23][C:24](=[O:25])[O:26][C:27]([CH3:28])([CH3:29])[CH3:30].O=[C:5](Cl)[CH2:4][CH2:3][O:2][CH3:1]>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][cH:12][cH:13][cH:14][c:15]3[c:1...
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.COCCC(=O)Cl
COCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
CO.C(Cl)Cl.CCO
Aromatic Heterocycle Formation
OtherReaction
2849961f1d737a23d71906fe74b0976730547255ac052bf4a7367ba2be72dd8e
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
90.8
[{"value": 90.8, "product": "COCCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (10.2 g, 29.5 mmol) in 250 mL of anhydrous CH2Cl2 was cooled to 0° C. and treated with triethylamine (4.18 mL, 30.0 mmol). Methoxypropionyl chloride (3.30 mL, 30.3 mmol) was then added dropwise over 5 min. The reaction was then warmed to r...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HCl
CO.C(Cl)Cl.CCO
null
1
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.COCCC(=O)Cl>CO.C(Cl)Cl.CCO>COCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5e6401fdcebf46d7b3a9fcdfea78a3c4
COCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1>>COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
COCCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O.ClC=1C=C(C(=O)OO)C=CC1>>COCCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O
[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31].O=C(O[OH:10])c1cccc(Cl)c1>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n+:9]([O-:10])[c:11]3[cH:12][cH:...
COCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1
COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)(Cl)Cl
Miscellaneous
OtherReaction
86abb75bf448eea8ddd78de30fcfc7b06bb61e46f725af6f1625e0dd9537993c
98b338a9d01476c0929fd5672e7509121bfe69600fd72e4d1cc6f1782e2d05d9
c1ccc2c(c1)[nH+]cc1nc[nH]c12
Cl-c1:c:c:c:c(-C(=O)-O-[OH;D1;+0:1]):c: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]
99.7
[{"value": 99.7, "product": "COCCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A solution of tert-butyl 2-{2-[2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethylcarbamate (10.22 g, 24.7 mmol) in 250 mL of CHCl3 was treated with 3-chloroperoxybenzoic acid (MCPBA, 77%, 9.12 g, 40.8 mmol). After stirring 30 min, the reaction mixture was washed with 1% Na2CO3 solution (2×75 mL) and brine. ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Peroxide
null
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(c[n+]c3ccccc32)[nH]1
HCl
C(Cl)(Cl)Cl
null
0.5
COCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1>C(Cl)(Cl)Cl>COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-02b41cb13ed44b7f9c6e44032ec7ef5f
COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>>COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
[NH4+].[OH-].COCCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O.[NH4+].[OH-].C(Cl)(Cl)Cl.C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(OC(C)(C)C)=O)CCOC
[O-][n+:10]1[cH:8][c:7]2[n:6][c:5]([CH2:4][CH2:3][O:2][CH3:1])[n:18]([CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31])[c:17]2[c:16]2[c:11]1[cH:12][cH:13][cH:14][cH:15]2.[NH4+:9]>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:1...
COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
ClCCCl
Protection
OtherReaction
1a3560ac88422fd247b995f02bc4ff4290625edd39947787fab7dac607ad70df
bf08eb59ebe808bce722373055de9689551bb60b2522898c82bc26646fc1fe40
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[n+;H0;D3:7](-[O-]):[c:8](:[c:9]):[c:10]:[c:11]:1:2.[NH4+;D0:12]>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:11]:1:[c:10]:[c:8](:[c:9]):[n;H0;D2;+0:7]:[c;H0;D3;+0:6]:2-[NH2;D1;+0:12]
null
[]
null
null
2
HOUR
A solution of tert-butyl 2-{2-[2-(2-methoxyethyl)-5-oxido-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethylcarbamate (10.6 g, 24.6 mmol) in 100 mL of 1,2-dichloroethane was heated to 60° C. and treated with 10 mL of concentrated NH4OH solution. To the rapidly stirred solution was added solid p-toluenesulfonyl chloride (7.05 ...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
ClCCCl
null
2
COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>ClCCCl>COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-af6fc172b955434b92c98e3db4a7fd5e
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1>>COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)CCOC.C1(=CC=CC=C1)N=C=O.CCN(CC)CC>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)CCOC
[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH2:24].[C:25](=[O:26])=[N:27][c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH...
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
null
null
C(Cl)Cl.CCOC(=O)C
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCOCCn1cnc2cnc3ccccc3c21)Nc1ccccc1
[C:1]-[C:2]-[NH2;D1;+0:3].[O;D1;H0:4]=[C;H0;D2;+0:5]=[N;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:5](=[O;D1;H0:4])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]
12.3
[{"value": 12.3, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)CCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
1-[2-(2-Aminoethoxy)ethyl]-2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-4-amine (750 mg, 2.28 mmol) was dissolved in 30 mL of anhydrous CH2Cl2 and cooled to 0° C. under N2. The reaction mixture was then treated with phenyl isocyanate (247 μL, 2.28 mmol) and Et3N (0.64 mL, 4.56 mmol) and allowed to warm slowly to room t...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
null
C(Cl)Cl.CCOC(=O)C
0
2
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1>C(Cl)Cl.CCOC(=O)C>COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a8d3be0f1d59427382222b78dfef6669
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN>>COCCc1nc2c(N)nc3c(c2n1CCOCCN)CCCC3
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)CCOC.[OH-].[Na+]>>NCCOCCN1C(=NC=2C(=NC=3CCCCC3C21)N)CCOC
[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[c:12]([c:13]2[n:14]1[CH2:15][CH2:16][O:17][CH2:18][CH2:19][NH2:20])[cH:21][cH:22][cH:23][cH:24]3>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[c:12]([c:13]2[n:14]1[CH2:15][CH2:16][O:17][CH2:18][CH2:19][NH2:20])[CH2:21][CH2:...
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN
COCCc1nc2c(N)nc3c(c2n1CCOCCN)CCCC3
null
O=[Pt]=O.O=[Pt]=O
O.FC(C(=O)O)(F)F
Reduction
OtherReaction
0e4a6a9a13d238c6a8679b2fe0694b39c5876b5c67afff3fabe8c9f8991c0ff5
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1nc2cnc3c(c2[nH]1)CCCC3
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:6]:[#7;a:7]:[c:8]3:[cH;D2;+0:9]:[cH;D2;+0:10]:[cH;D2;+0:11]:[cH;D2;+0:12]:[c:13]:3:[c:14]:1:2>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:6]:[#7;a:7]:[c:8]3:[c:13](:[c:14]:1:2)-[CH2;D2;+0:12]-[CH2;D2;+0:11]-[CH2;D2;+0:10]-[CH2;D2;+0:9]-3
56.8
[{"value": 56.8, "product": "NCCOCCN1C(=NC=2C(=NC=3CCCCC3C21)N)CCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
DAY
1-[2-(2-Aminoethoxy)ethyl]-2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-4-amine (10.0 g, 27.3 mmol) was dissolved in 50 mL of trifluoroacetic acid and treated with PtO2 (1.0 g). The reaction mixture was shaken under H2 (3 Kg/cm2). After 4 d, an additional 0.5 g of PtO2 was added and hydrogenation was continued for an a...
10.6084/m9.figshare.5104873.v1
null
null
null
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c3c(ncc2[nH]1)CCCC3
c1nc2c3c(ncc2[nH]1)CCCC3
null
O=[Pt]=O.O=[Pt]=O.O.FC(C(=O)O)(F)F
null
96
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN>O=[Pt]=O.O=[Pt]=O.O.FC(C(=O)O)(F)F>COCCc1nc2c(N)nc3c(c2n1CCOCCN)CCCC3
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dad8df40988e4f31b87f0a164dd34f68
COCCc1nc2c(N)nc3c(c2n1CCOCCN)CCCC3.O=C=Nc1ccccc1>>COCCc1nc2c(N)nc3c(c2n1CCOCCNC(=O)Nc1ccccc1)CCCC3
NCCOCCN1C(=NC=2C(=NC=3CCCCC3C21)N)CCOC.C1(=CC=CC=C1)N=C=O.CCN(CC)CC>>NC1=NC=2CCCCC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)CCOC
[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[c:12]([c:13]2[n:14]1[CH2:15][CH2:16][O:17][CH2:18][CH2:19][NH2:20])[CH2:30][CH2:31][CH2:32][CH2:33]3.[C:21](=[O:22])=[N:23][c:24]1[cH:25][cH:26][cH:27][cH:28][cH:29]1>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[c:12]([c:1...
COCCc1nc2c(N)nc3c(c2n1CCOCCN)CCCC3.O=C=Nc1ccccc1
COCCc1nc2c(N)nc3c(c2n1CCOCCNC(=O)Nc1ccccc1)CCCC3
null
null
C(Cl)Cl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCOCCn1cnc2cnc3c(c21)CCCC3)Nc1ccccc1
[C:1]-[C:2]-[NH2;D1;+0:3].[O;D1;H0:4]=[C;H0;D2;+0:5]=[N;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:5](=[O;D1;H0:4])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]
36.8
[{"value": 36.8, "product": "NC1=NC=2CCCCC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)CCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
8
HOUR
1-[2-(2-Aminoethoxy)ethyl]-2-(2-methoxyethyl)-6,7,8,9-tetrahydro-1H-imidazo[4,5-c]quinolin-4-amine (919 mg, 2.76 mmol) was dissolved in 30 mL of anhydrous CH2Cl2 and cooled to 0° C. under N2. The reaction mixture was then treated with phenyl isocyanate (300 μL, 2.76 mmol) and Et3N (0.77 mL, 5.51 mmol) and allowed to wa...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1nc2c3c(ncc2[nH]1)CCCC3
null
C(Cl)Cl
0
8
COCCc1nc2c(N)nc3c(c2n1CCOCCN)CCCC3.O=C=Nc1ccccc1>C(Cl)Cl>COCCc1nc2c(N)nc3c(c2n1CCOCCNC(=O)Nc1ccccc1)CCCC3
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-025aabda249041eaa8d627746d8fa17c
CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-].CI>>CN(CCOCCN=[N+]=[N-])C(=O)OC(C)(C)C
CI.[H-].[Na+].N(=[N+]=[N-])CCOCCNC(OC(C)(C)C)=O.[H-].[Na+]>>N(=[N+]=[N-])CCOCCN(C(OC(C)(C)C)=O)C
[NH:2]([CH2:3][CH2:4][O:5][CH2:6][CH2:7][N:8]=[N+:9]=[N-:10])[C:11](=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[CH3:17].I[CH3:1]>>[CH3:1][N:2]([CH2:3][CH2:4][O:5][CH2:6][CH2:7][N:8]=[N+:9]=[N-:10])[C:11](=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[CH3:17]
CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-].CI
CN(CCOCCN=[N+]=[N-])C(=O)OC(C)(C)C
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
29c841ae076cb6ee785aad2a4e3ce1a9b47357d7ad25657b8d9991b1347f5721
c485eddcb40c5a0d396ffdb624041effa09ee4f5ca2ecce3fe13077cf65004ed
null
I-[CH3;D1;+0:1].[C:2]-[C:3]-[NH;D2;+0:4]-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:11]>>[C:2]-[C:3]-[N;H0;D3;+0:4](-[CH3;D1;+0:1])-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:11]
94.2
[{"value": 94.2, "product": "N(=[N+]=[N-])CCOCCN(C(OC(C)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
Sodium hydride (60% oil dispersion, 9.1 g, 228 mmol) was placed in a round bottom flask and washed with hexanes (3×) under N2. The dried sodium hydride was treated with 800 mL of anhydrous THF. A solution of tert-butyl 2-(2-azidoethoxy)ethylcarbamate (41.9 g, 182 mmol) in 200 mL of THF was then added to the stirred sod...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester
Carbamic ester
null
null
null
HI
C1CCOC1
null
0.333333
CC(C)(C)OC(=O)NCCOCCN=[N+]=[N-].CI>C1CCOC1>CN(CCOCCN=[N+]=[N-])C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dc29b9fde43c4a0abefb56f46251793a
CN(CCOCCN=[N+]=[N-])C(=O)OC(C)(C)C>>CN(CCOCCN)C(=O)OC(C)(C)C
N(=[N+]=[N-])CCOCCN(C(OC(C)(C)C)=O)C>>NCCOCCN(C(OC(C)(C)C)=O)C
[N-]=[N+]=[N:8][CH2:7][CH2:6][O:5][CH2:4][CH2:3][N:2]([CH3:1])[C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15]>>[CH3:1][N:2]([CH2:3][CH2:4][O:5][CH2:6][CH2:7][NH2:8])[C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15]
CN(CCOCCN=[N+]=[N-])C(=O)OC(C)(C)C
CN(CCOCCN)C(=O)OC(C)(C)C
null
[Pd]
CO
Reduction
Azide to amine reduction (Staudinger)
4c9e4990dae2bb965dec06bd45e318560989ee3681b61e443f7aa363b7cfa222
cd009d687d606bf351eac9390a176d16be38f2c8216a599b398641009c215027
null
[C:1]-[C:2]-[N;H0;D2;+0:3]=[N+]=[N-]>>[C:1]-[C:2]-[NH2;D1;+0:3]
100.2
[{"value": 100.2, "product": "NCCOCCN(C(OC(C)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution tert-butyl 2-(2-azidoethoxy)ethyl(methyl)carbamate (41.9 g, 170 mmol) in 600 mL of MeOH was treated with 2.5 g of 10% Pd on carbon and shaken under H2 (3 Kg/cm2) for 24 h. The solution was then filtered through a Celite pad and concentrated to give 37.2 g of crude tert-butyl 2-(2-aminoethoxy)ethyl(methyl)car...
10.6084/m9.figshare.5104873.v1
null
Azide
Primary amine
null
null
null
Other
[Pd].CO
null
24
CN(CCOCCN=[N+]=[N-])C(=O)OC(C)(C)C>[Pd].CO>CN(CCOCCN)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c88ac23e2154438b9ed5a2f01284f5d4
CN(CCOCCN)C(=O)OC(C)(C)C.O=[N+]([O-])c1cnc2ccccc2c1Cl>>CN(CCOCCNc1c([N+](=O)[O-])cnc2ccccc12)C(=O)OC(C)(C)C
ClC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-].C(C)N(CC)CC.NCCOCCN(C(OC(C)(C)C)=O)C>>CN(C(OC(C)(C)C)=O)CCOCCNC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]
[CH3:1][N:2]([CH2:3][CH2:4][O:5][CH2:6][CH2:7][NH2:8])[C:22](=[O:23])[O:24][C:25]([CH3:26])([CH3:27])[CH3:28].Cl[c:9]1[c:10]([N+:11](=[O:12])[O-:13])[cH:14][n:15][c:16]2[cH:17][cH:18][cH:19][cH:20][c:21]12>>[CH3:1][N:2]([CH2:3][CH2:4][O:5][CH2:6][CH2:7][NH:8][c:9]1[c:10]([N+:11](=[O:12])[O-:13])[cH:14][n:15][c:16]2[cH:...
CN(CCOCCN)C(=O)OC(C)(C)C.O=[N+]([O-])c1cnc2ccccc2c1Cl
CN(CCOCCNc1c([N+](=O)[O-])cnc2ccccc12)C(=O)OC(C)(C)C
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2ncccc2c1
Cl-[c;H0;D3;+0:1]1:[c:2](-[#7;+:3]):[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8]:1:[c:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:3]-[c:2]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
77.2
[{"value": 77.2, "product": "CN(C(OC(C)(C)C)=O)CCOCCNC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A stirred solution of 4-chloro-3-nitroquinoline (32.3 g, 155 mmol) in 400 mL of anhydrous CH2Cl2, under N2, was treated with triethylamine (43.1 mL, 310 mmol) and tert-butyl 2-(2-aminoethoxy)ethyl(methyl)carbamate (37.2 g, 171 mmol). After stirring overnight, the reaction mixture was washed with H2O (2×300 mL) and brin...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
C(Cl)Cl
null
8
CN(CCOCCN)C(=O)OC(C)(C)C.O=[N+]([O-])c1cnc2ccccc2c1Cl>C(Cl)Cl>CN(CCOCCNc1c([N+](=O)[O-])cnc2ccccc12)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-790bffd1a5474b7e9bddf9f4c3316e68
CN(CCOCCNc1c([N+](=O)[O-])cnc2ccccc12)C(=O)OC(C)(C)C>>CN(CCOCCNc1c(N)cnc2ccccc12)C(=O)OC(C)(C)C
CN(C(OC(C)(C)C)=O)CCOCCNC1=C(C=NC2=CC=CC=C12)[N+](=O)[O-]>>NC=1C=NC2=CC=CC=C2C1NCCOCCN(C(OC(C)(C)C)=O)C
O=[N+:11]([O-])[c:10]1[c:9]([NH:8][CH2:7][CH2:6][O:5][CH2:4][CH2:3][N:2]([CH3:1])[C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[c:19]2[c:14]([n:13][cH:12]1)[cH:15][cH:16][cH:17][cH:18]2>>[CH3:1][N:2]([CH2:3][CH2:4][O:5][CH2:6][CH2:7][NH:8][c:9]1[c:10]([NH2:11])[cH:12][n:13][c:14]2[cH:15][cH:16][cH:17][cH:18][...
CN(CCOCCNc1c([N+](=O)[O-])cnc2ccccc12)C(=O)OC(C)(C)C
CN(CCOCCNc1c(N)cnc2ccccc12)C(=O)OC(C)(C)C
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]
112.3
[{"value": 112.3, "product": "NC=1C=NC2=CC=CC=C2C1NCCOCCN(C(OC(C)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution of tert-butyl methyl(2-{2-[(3-nitroquinolin-4-yl)amino]ethoxy}ethyl)carbamate (6.56 g, 16.8 mmol) in 75 mL of toluene was treated with 0.5 g of 5% Pt on carbon and shaken under H2 (3 Kg/cm2) for 24 h. The solution was then filtered through a Celite pad and concentrated to give 6.8 g of crude tert-butyl 2-{2-...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C1(=CC=CC=C1)C
null
24
CN(CCOCCNc1c([N+](=O)[O-])cnc2ccccc12)C(=O)OC(C)(C)C>[Pt].C1(=CC=CC=C1)C>CN(CCOCCNc1c(N)cnc2ccccc12)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1ace2d11d6e444918f7af8a4b0dc9206
CN(CCOCCNc1c(N)cnc2ccccc12)C(=O)OC(C)(C)C.COCCC(=O)Cl>>COCCc1nc2cnc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
C.COCCC(=O)Cl.C(C)N(CC)CC.NC=1C=NC2=CC=CC=C2C1NCCOCCN(C(OC(C)(C)C)=O)C.C(C)N(CC)CC>>COCCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCN(C(OC(C)(C)C)=O)C
[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1[NH:17][CH2:18][CH2:19][O:20][CH2:21][CH2:22][N:23]([CH3:24])[C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31].O=[C:5](Cl)[CH2:4][CH2:3][O:2][CH3:1]>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][cH:12][cH:13][cH:14][c...
CN(CCOCCNc1c(N)cnc2ccccc12)C(=O)OC(C)(C)C.COCCC(=O)Cl
COCCc1nc2cnc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
null
null
CO.C(Cl)Cl.CCO
Aromatic Heterocycle Formation
OtherReaction
2849961f1d737a23d71906fe74b0976730547255ac052bf4a7367ba2be72dd8e
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
100
[{"value": 100.0, "product": "COCCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCN(C(OC(C)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethyl(methyl)carbamate (6.05 g, 16.8 mmol) in 200 mL of anhydrous CH2Cl2 was cooled to 0° C. and treated with triethylamine (2.40 mL, 17.2 mmol). Methoxypropionyl chloride (1.72 mL, 17.2 mmol) was then added dropwise over 5 min. The reaction was then war...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HCl
CO.C(Cl)Cl.CCO
null
3
CN(CCOCCNc1c(N)cnc2ccccc12)C(=O)OC(C)(C)C.COCCC(=O)Cl>CO.C(Cl)Cl.CCO>COCCc1nc2cnc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-da69ac99ee0a4b629e7ceb03ac1c3e56
COCCc1nc2cnc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1>>COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
C(=O)(O)[O-].[Na+].COCCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCN(C(OC(C)(C)C)=O)C.C1=CC(=CC(=C1)Cl)C(=O)OO>>COCCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCN(C(OC(C)(C)C)=O)C
[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][N:24]([CH3:25])[C:26](=[O:27])[O:28][C:29]([CH3:30])([CH3:31])[CH3:32].O=C(O[OH:10])c1cccc(Cl)c1>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n+:9]([O-:10])[c:11]3[c...
COCCc1nc2cnc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1
COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
86abb75bf448eea8ddd78de30fcfc7b06bb61e46f725af6f1625e0dd9537993c
98b338a9d01476c0929fd5672e7509121bfe69600fd72e4d1cc6f1782e2d05d9
c1ccc2c(c1)[nH+]cc1nc[nH]c12
Cl-c1:c:c:c:c(-C(=O)-O-[OH;D1;+0:1]):c: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]
94.4
[{"value": 94.4, "product": "COCCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCN(C(OC(C)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
6
HOUR
A solution of tert-butyl 2-{2-[2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethyl(methyl)carbamate (7.20 g, 16.8 mmol) in 200 mL of CH2Cl2 was treated with MCPBA (77%, 4.32 g, 19.3 mmol). After stirring 6 h, the reaction mixture was treated with saturated NaHCO3 solution and the layers were separated. The o...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Peroxide
null
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(c[n+]c3ccccc32)[nH]1
HCl
C(Cl)Cl
null
6
COCCc1nc2cnc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1>C(Cl)Cl>COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9764a74295d040ab920405ed2f5f78a5
COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C.[NH4+]>>COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
[NH4+].[OH-].COCCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCN(C(OC(C)(C)C)=O)C.[NH4+].[OH-].C(Cl)Cl.C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCN(C(OC(C)(C)C)=O)C)CCOC
[O-][n+:10]1[cH:8][c:7]2[n:6][c:5]([CH2:4][CH2:3][O:2][CH3:1])[n:18]([CH2:19][CH2:20][O:21][CH2:22][CH2:23][N:24]([CH3:25])[C:26](=[O:27])[O:28][C:29]([CH3:30])([CH3:31])[CH3:32])[c:17]2[c:16]2[c:11]1[cH:12][cH:13][cH:14][cH:15]2.[NH4+:9]>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH...
COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C.[NH4+]
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
null
null
ClCCCl
Protection
OtherReaction
1a3560ac88422fd247b995f02bc4ff4290625edd39947787fab7dac607ad70df
bf08eb59ebe808bce722373055de9689551bb60b2522898c82bc26646fc1fe40
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[n+;H0;D3:7](-[O-]):[c:8](:[c:9]):[c:10]:[c:11]:1:2.[NH4+;D0:12]>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:11]:1:[c:10]:[c:8](:[c:9]):[n;H0;D2;+0:7]:[c;H0;D3;+0:6]:2-[NH2;D1;+0:12]
null
[]
null
null
4
HOUR
A solution of tert-butyl 2-{2-[2-(2-methoxyethyl)-5-oxido-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethyl(methyl)carbamate (7.05 g, 15.9 mmol) in 100 mL of 1,2-dichloroethane was heated to 80° C. and treated with 5 mL of concentrated NH4OH solution. To the rapidly stirred solution was added solid p-toluenesulfonyl chloride...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
ClCCCl
null
4
COCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C.[NH4+]>ClCCCl>COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN(C)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-91a696e50c514cf2be058a01532b86ef
CNCCOCCn1c(CCOC)nc2c(N)nc3ccccc3c21>>CNCCOCCn1c(CCOC)nc2c(N)nc3c(c21)CCCC3
COCCC=1N(C2=C(C(=NC=3C=CC=CC23)N)N1)CCOCCNC>>COCCC=1N(C2=C(C(=NC=3CCCCC23)N)N1)CCOCCNC
[CH3:1][NH:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][n:8]1[c:9]([CH2:10][CH2:11][O:12][CH3:13])[n:14][c:15]2[c:16]([NH2:17])[n:18][c:19]3[c:20]([c:21]12)[cH:22][cH:23][cH:24][cH:25]3>>[CH3:1][NH:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][n:8]1[c:9]([CH2:10][CH2:11][O:12][CH3:13])[n:14][c:15]2[c:16]([NH2:17])[n:18][c:19]3[c:20]([c:2...
CNCCOCCn1c(CCOC)nc2c(N)nc3ccccc3c21
CNCCOCCn1c(CCOC)nc2c(N)nc3c(c21)CCCC3
null
O=[Pt]=O.O=[Pt]=O
O.FC(C(=O)O)(F)F
Reduction
OtherReaction
8818364208f28bd8959a2ecaa0a3d40df79a7089572c5d620cd44005e9183ac2
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1nc2cnc3c(c2[nH]1)CCCC3
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:6]:[#7;a:7]:[c:8]3:[cH;D2;+0:9]:[cH;D2;+0:10]:[cH;D2;+0:11]:[cH;D2;+0:12]:[c:13]:3:[c:14]:1:2>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:6]:[#7;a:7]:[c:8]3:[c:13](:[c:14]:1:2)-[CH2;D2;+0:12]-[CH2;D2;+0:11]-[CH2;D2;+0:10]-[CH2;D2;+0:9]-3
74.6
[{"value": 74.6, "product": "COCCC=1N(C2=C(C(=NC=3CCCCC23)N)N1)CCOCCNC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
DAY
2-(2-Methoxyethyl)-1-{2-[2-(methylamino)ethoxy]ethyl}-1H-imidazo[4,5-c]quinolin-4-amine (4.22 g, 12.3 mmol) was dissolved in 25 mL of trifluoroacetic acid and treated with PtO2 (0.5 g). The reaction mixture was shaken under H2 (3 Kg/cm2). After 4 d, an additional 0.5 g of PtO2 was added and hydrogenation was continued ...
10.6084/m9.figshare.5104873.v1
null
null
null
c1nc2cnc3ccccc3c2[nH]1
c1nc2cnc3c(c2[nH]1)CCCC3
c1nc2cnc3c(c2[nH]1)CCCC3
null
O=[Pt]=O.O=[Pt]=O.O.FC(C(=O)O)(F)F
null
96
CNCCOCCn1c(CCOC)nc2c(N)nc3ccccc3c21>O=[Pt]=O.O=[Pt]=O.O.FC(C(=O)O)(F)F>CNCCOCCn1c(CCOC)nc2c(N)nc3c(c21)CCCC3
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5898e3f28521491e8bd3281da6e64dd3
CNCCOCCn1c(CCOC)nc2c(N)nc3c(c21)CCCC3.O=C=Nc1ccccc1>>COCCc1nc2c(N)nc3c(c2n1CCOCCN(C)C(=O)Nc1ccccc1)CCCC3
COCCC=1N(C2=C(C(=NC=3CCCCC23)N)N1)CCOCCNC.C1(=CC=CC=C1)N=C=O>>NC1=NC=2CCCCC2C2=C1N=C(N2CCOCCN(C(=O)NC2=CC=CC=C2)C)CCOC
[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[c:12]([c:13]2[n:14]1[CH2:15][CH2:16][O:17][CH2:18][CH2:19][NH:20][CH3:21])[CH2:31][CH2:32][CH2:33][CH2:34]3.[C:22](=[O:23])=[N:24][c:25]1[cH:26][cH:27][cH:28][cH:29][cH:30]1>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[c:1...
CNCCOCCn1c(CCOC)nc2c(N)nc3c(c21)CCCC3.O=C=Nc1ccccc1
COCCc1nc2c(N)nc3c(c2n1CCOCCN(C)C(=O)Nc1ccccc1)CCCC3
null
null
C(Cl)Cl
Acylation
Urea synthesis via isocyanate and secondary amine
288f31369c46060b9009e57afc96d52a76d6a0243a2e1197ab47b0221bb8a3ee
5272a383a93723269f1934f97993b0175b43cd993bcdf2f45add1dbb852d1e09
O=C(NCCOCCn1cnc2cnc3c(c21)CCCC3)Nc1ccccc1
[C:1]-[C:2]-[NH;D2;+0:3]-[C;D1;H3:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[c:8](:[c:9]):[c:10]>>[C:1]-[C:2]-[N;H0;D3;+0:3](-[C;D1;H3:4])-[C;H0;D3;+0:6](=[O;D1;H0:5])-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10]
16.9
[{"value": 16.9, "product": "NC1=NC=2CCCCC2C2=C1N=C(N2CCOCCN(C(=O)NC2=CC=CC=C2)C)CCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
2-(2-Methoxyethyl)-1-{2-[2-(methylamino)ethoxy]ethyl}-6,7,8,9-tetrahydro-1H-imidazo[4,5-c]quinolin-4-amine (750 mg, 2.16 mmol) was dissolved in 30 mL of anhydrous CH2Cl2 and treated with phenyl isocyanate (239 μL, 2.20 mmol). After stirring under N2 overnight, the reaction mixture was concentrated under reduced pressur...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Secondary amine
Urea
null
null
c1ccccc1.c1nc2c3c(ncc2[nH]1)CCCC3
null
C(Cl)Cl
null
8
CNCCOCCn1c(CCOC)nc2c(N)nc3c(c21)CCCC3.O=C=Nc1ccccc1>C(Cl)Cl>COCCc1nc2c(N)nc3c(c2n1CCOCCN(C)C(=O)Nc1ccccc1)CCCC3
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c58d06a7b15144a099e79e0c7977f05d
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1>>COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)CCOC.C(C)N(CC)CC.N1(CCOCC1)C(=O)Cl>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)N2CCOCC2)CCOC
[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH2:24].Cl[C:25](=[O:26])[N:27]1[CH2:28][CH2:29][O:30][CH2:31][CH2:32]1>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:1...
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
null
null
ClCCl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
b81fefae7607aa106605114867756af2924064950a2aea97200543849613e96a
406c5893488430105533c87dfb5d625d8382e709e047cda9cfdc2235e742a9cf
O=C(NCCOCCn1cnc2cnc3ccccc3c21)N1CCOCC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C:4])-[C:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C:4])-[C:5]
19.7
[{"value": 19.7, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)N2CCOCC2)CCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
Under a nitrogen atmosphere, 1-[2-(2-aminoethoxy)ethyl]-2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-4-amine (0.75 g, 2.3 mmol) was dissolved in dichloromethane (30 mL) and triethylamine (0.64 mL, 4.6 mmol) using mild heat and vigorous stirring. The solution was chilled in an ice-water bath and 4-morpholinecarbonyl chl...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Tertiary amide.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.C1COCC[NH]1
HCl
ClCCl
null
4
COCCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1>ClCCl>COCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f879e33c6a214b28b948da2d4183ca18
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCCCC(OCC)(OCC)OCC>>CCCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
C.Cl.[NH+]1=CC=CC=C1.NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O.C(C)OC(CCCC)(OCC)OCC>>C(CCC)C=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O
[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1[NH:17][CH2:18][CH2:19][O:20][CH2:21][CH2:22][NH:23][C:24](=[O:25])[O:26][C:27]([CH3:28])([CH3:29])[CH3:30].CCO[C:5](OCC)(OCC)[CH2:4][CH2:3][CH2:2][CH3:1]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][cH:12][cH:13][cH:14]...
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCCCC(OCC)(OCC)OCC
CCCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C1(=CC=CC=C1)C.CO
Aromatic Heterocycle Formation
OtherReaction
af7d6de7ca5153ecd31a13d7075f2969261301df4b656bfec36bc67fd1ea176b
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc2c(c1)ncc1nc[nH]c12
C-C-O-[C;H0;D4;+0:1](-O-C-C)(-O-C-C)-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
99.9
[{"value": 99.9, "product": "C(CCC)C=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (3.46 g, 10.0 mmol) in 50 mL of toluene was treated with triethylorthovalerate (2.5 mL, 14.5 mmol) and the reaction mixture was heated to reflux. A 25 mg portion of pyridinium hydrochloride was then added and refluxing was continued for 4 ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
C1(=CC=CC=C1)C.CO
null
4
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCCCC(OCC)(OCC)OCC>C1(=CC=CC=C1)C.CO>CCCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-607cc0f0838b42f2b1ca3aaabc9a99b1
CCCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1>>CCCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
C(=O)(O)[O-].[Na+].C(CCC)C=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O.ClC=1C=C(C(=O)OO)C=CC1>>C(CCC)C=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O
[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31].O=C(O[OH:10])c1cccc(Cl)c1>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n+:9]([O-:10])[c:11]3[cH:12]...
CCCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1
CCCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
86abb75bf448eea8ddd78de30fcfc7b06bb61e46f725af6f1625e0dd9537993c
98b338a9d01476c0929fd5672e7509121bfe69600fd72e4d1cc6f1782e2d05d9
c1ccc2c(c1)[nH+]cc1nc[nH]c12
Cl-c1:c:c:c:c(-C(=O)-O-[OH;D1;+0:1]):c: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]
85.9
[{"value": 85.9, "product": "C(CCC)C=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
A solution of tert-butyl 2-[2-(2-butyl-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (4.12 g, 10.0 mmol) in 50 mL of CH2Cl2 was treated with 3-chloroperoxybenzoic acid (MCPBA, 77%, 2.5 g, 11.2 mmol). After stirring for 5 h, the reaction mixture was treated with saturated NaHCO3 solution and the layers were separ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Peroxide
null
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(c[n+]c3ccccc32)[nH]1
HCl
C(Cl)Cl
null
5
CCCCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1>C(Cl)Cl>CCCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4d0031d66259482c8a402873a60126a9
CCCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>>CCCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
C(Cl)Cl.[NH4+].[OH-].C(CCC)C=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O.C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(OC(C)(C)C)=O)CCCC
[O-][n+:10]1[cH:8][c:7]2[n:6][c:5]([CH2:4][CH2:3][CH2:2][CH3:1])[n:18]([CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31])[c:17]2[c:16]2[c:11]1[cH:12][cH:13][cH:14][cH:15]2.[NH4+:9]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][...
CCCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]
CCCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
ClCCCl
Protection
OtherReaction
1a3560ac88422fd247b995f02bc4ff4290625edd39947787fab7dac607ad70df
bf08eb59ebe808bce722373055de9689551bb60b2522898c82bc26646fc1fe40
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[n+;H0;D3:7](-[O-]):[c:8](:[c:9]):[c:10]:[c:11]:1:2.[NH4+;D0:12]>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:11]:1:[c:10]:[c:8](:[c:9]):[n;H0;D2;+0:7]:[c;H0;D3;+0:6]:2-[NH2;D1;+0:12]
null
[]
null
null
2
HOUR
A solution of tert-butyl 2-[2-(2-butyl-5-oxido-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (3.68 g, 8.60 mmol) in 100 mL of 1,2-dichloroethane was heated to 80° C. and treated with 10 mL of concentrated NH4OH solution. To the rapidly stirred solution was added solid p-toluenesulfonyl chloride (1.87 g, 9.81 mmo...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
ClCCCl
null
2
CCCCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>ClCCCl>CCCCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e01dd0b85c3048c5994888a54ce6b1ba
CC(C)(C)OC(=O)N1CCC(CCI)CC1.CCC(CO)n1cnc2cnc3ccccc3c21>>CCC(COCCC1CCN(C(=O)OC(C)(C)C)CC1)n1cnc2cnc3ccccc3c21
[Cl-].[NH4+].N1(C=NC=2C=NC=3C=CC=CC3C21)C(CO)CC.[H-].[Na+].ICCC1CCN(CC1)C(=O)OC(C)(C)C>>N1(C=NC=2C=NC=3C=CC=CC3C21)C(COCCC2CCN(CC2)C(=O)OC(C)(C)C)CC
I[CH2:6][CH2:7][CH:8]1[CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]1.[CH3:1][CH2:2][CH:3]([CH2:4][OH:5])[n:21]1[cH:22][n:23][c:24]2[cH:25][n:26][c:27]3[cH:28][cH:29][cH:30][cH:31][c:32]3[c:33]12>>[CH3:1][CH2:2][CH:3]([CH2:4][O:5][CH2:6][CH2:7][CH:8]1[CH2:9][CH2:10][N:11]...
CC(C)(C)OC(=O)N1CCC(CCI)CC1.CCC(CO)n1cnc2cnc3ccccc3c21
CCC(COCCC1CCN(C(=O)OC(C)(C)C)CC1)n1cnc2cnc3ccccc3c21
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
dd3f9c60e1f90d961a7c01d970ae213561355ee1451f276a3b04696e4b6fae5c
46a6e883cf919b4006e69abfdfd883f458f55c08b3200960c6a5b57c4139fbca
c1ccc2c(c1)ncc1ncn(CCOCCC3CCNCC3)c12
I-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[C:5]-[OH;D1;+0:6]>>[C:4]-[C:5]-[O;H0;D2;+0:6]-[CH2;D2;+0:1]-[C:2]-[C:3]
18.1
[{"value": 18.1, "product": "N1(C=NC=2C=NC=3C=CC=CC3C21)C(COCCC2CCN(CC2)C(=O)OC(C)(C)C)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
45
MINUTE
Under a nitrogen atmosphere, 2-(1H-imidazo[4,5-c]quinolin-1-yl)butan-1-ol (6.5 g, 26.9 mmol) was added in three portions to a suspension of sodium hydride (1.4 g of 60%, 35.0 mmol) in anhydrous N,N-dimethylformamide. The reaction mixture was allowed to stir for 45 minutes by which time gas evolution had ceased. Tert-bu...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary alcohol
Ether
null
null
C1CC[NH]CC1.c1ccc2c(c1)ncc1nc[nH]c12
HI
CN(C=O)C
100
0.75
CC(C)(C)OC(=O)N1CCC(CCI)CC1.CCC(CO)n1cnc2cnc3ccccc3c21>CN(C=O)C>CCC(COCCC1CCN(C(=O)OC(C)(C)C)CC1)n1cnc2cnc3ccccc3c21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-415921c8e7b844f19c8c633e71c1e7dc
CCC(COCCC1CCN(C(=O)OC(C)(C)C)CC1)n1cnc2c(N)nc3ccccc3c21>>CCC(COCCC1CCNCC1)n1cnc2c(N)nc3ccccc3c21
NC1=NC=2C=CC=CC2C2=C1N=CN2C(COCCC2CCN(CC2)C(=O)OC(C)(C)C)CC.Cl>>N1CCC(CC1)CCOCC(CC)N1C=NC=2C(=NC=3C=CC=CC3C21)N
CC(C)(C)OC(=O)[N:11]1[CH2:10][CH2:9][CH:8]([CH2:7][CH2:6][O:5][CH2:4][CH:3]([CH2:2][CH3:1])[n:14]2[cH:15][n:16][c:17]3[c:18]([NH2:19])[n:20][c:21]4[cH:22][cH:23][cH:24][cH:25][c:26]4[c:27]23)[CH2:13][CH2:12]1>>[CH3:1][CH2:2][CH:3]([CH2:4][O:5][CH2:6][CH2:7][CH:8]1[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1)[n:14]1[cH:15][n...
CCC(COCCC1CCN(C(=O)OC(C)(C)C)CC1)n1cnc2c(N)nc3ccccc3c21
CCC(COCCC1CCNCC1)n1cnc2c(N)nc3ccccc3c21
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc2c(c1)ncc1ncn(CCOCCC3CCNCC3)c12
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:5]-[C:4]-[NH;D2;+0:1]-[C:2]-[C:3]
64.8
[{"value": 64.8, "product": "N1CCC(CC1)CCOCC(CC)N1C=NC=2C(=NC=3C=CC=CC3C21)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
14
HOUR
Under a nitrogen atmosphere, tert-butyl 4-{2-[2-(4-amino-1H-imidazo[4,5-c]quinolin-1-yl)butoxy]ethyl}piperidine-1-carboxylate (1.00 g, 2.1 mmol) and 2N ethanolic hydrochloric acid (10 ml, 20 mmol) were combined and the solution was stirred at ambient temperature for 14 hours. The solvent was removed in vacuo and the re...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1.c1nc2ccccc2c2[nH]cnc12
HO-
null
null
14
CCC(COCCC1CCN(C(=O)OC(C)(C)C)CC1)n1cnc2c(N)nc3ccccc3c21>>CCC(COCCC1CCNCC1)n1cnc2c(N)nc3ccccc3c21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a71453b19c6d45048d89d67e928352f6
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12>>CC(C)(C)OC(=O)NCCOCCn1cnc2cnc3ccccc3c21
C.Cl.[NH+]1=CC=CC=C1.NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O.C(C)OC(OCC)OCC>>N1(C=NC=2C=NC=3C=CC=CC3C21)CCOCCNC(OC(C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][NH:14][c:26]1[c:17]([NH2:16])[cH:18][n:19][c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]21>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][n:14]1[cH:15][n:16][c:17]2[cH:18][n:19][c:20]3[cH...
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12
CC(C)(C)OC(=O)NCCOCCn1cnc2cnc3ccccc3c21
null
null
C1(=CC=CC=C1)C.CO
Aromatic Heterocycle Formation
OtherReaction
26779edfcc2b370e3e3dc285e0fedfbcf04e6b6c7fd46f2674bab3f061a7b270
c12bf4e666f812d0e692aca3756678364265d1c8b3469e9563c84f9ed1df94d2
c1ccc2c(c1)ncc1nc[nH]c12
[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
73.6
[{"value": 73.6, "product": "N1(C=NC=2C=NC=3C=CC=CC3C21)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (6.92 g, 20.0 mmol) in 100 mL of toluene was treated with triethylorthoformate (4.65 mL, 28.0 mmol) and the reaction mixture was heated to reflux. A 100 mg portion of pyridinium hydrochloride was then added and refluxing was continued for ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1nc[nH]c12
c1ccc2c(c1)ncc1nc[nH]c12
Other
C1(=CC=CC=C1)C.CO
null
2
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12>C1(=CC=CC=C1)C.CO>CC(C)(C)OC(=O)NCCOCCn1cnc2cnc3ccccc3c21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3fbe7793ca8944c990104b91c939d97c
CC(C)(C)OC(=O)NCCOCCn1cnc2cnc3ccccc3c21.O=C(OO)c1cccc(Cl)c1>>CC(C)(C)OC(=O)NCCOCCn1cnc2c[n+]([O-])c3ccccc3c21
C(=O)(O)[O-].[Na+].N1(C=NC=2C=NC=3C=CC=CC3C21)CCOCCNC(OC(C)(C)C)=O.C1=CC(=CC(=C1)Cl)C(=O)OO>>[O-][N+]1=CC2=C(C=3C=CC=CC13)N(C=N2)CCOCCNC(OC(C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][n:14]1[cH:15][n:16][c:17]2[cH:18][n:19][c:21]3[cH:22][cH:23][cH:24][cH:25][c:26]3[c:27]12.O=C(O[OH:20])c1cccc(Cl)c1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][n:14]1[cH:15][n:16]...
CC(C)(C)OC(=O)NCCOCCn1cnc2cnc3ccccc3c21.O=C(OO)c1cccc(Cl)c1
CC(C)(C)OC(=O)NCCOCCn1cnc2c[n+]([O-])c3ccccc3c21
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
cad786c9409a25c8ce82607722e58ecf517f297ff4b081be9d5601c67b613c7c
98b338a9d01476c0929fd5672e7509121bfe69600fd72e4d1cc6f1782e2d05d9
c1ccc2c(c1)[nH+]cc1nc[nH]c12
Cl-c1:c:c:c:c(-C(=O)-O-[OH;D1;+0:1]):c: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]
84
[{"value": 84.0, "product": "[O-][N+]1=CC2=C(C=3C=CC=CC13)N(C=N2)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of tert-butyl 2-[2-(1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (5.25 g, 14.7 mmol) in 200 mL of CH2Cl2 was treated with MCPBA (77%, 3.63 g, 16.3 mmol). After stirring overnight, the reaction mixture was treated with saturated NaHCO3 solution and the layers were separated. The organic portion was wa...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Peroxide
null
c1ccc2c(c1)ncc1nc[nH]c12.c1ccccc1
c1ccc2c(c1)[n+]cc1nc[nH]c12
c1ccc2c(c1)[n+]cc1nc[nH]c12
HCl
C(Cl)Cl
null
8
CC(C)(C)OC(=O)NCCOCCn1cnc2cnc3ccccc3c21.O=C(OO)c1cccc(Cl)c1>C(Cl)Cl>CC(C)(C)OC(=O)NCCOCCn1cnc2c[n+]([O-])c3ccccc3c21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-be86840fafae4e68922eca13ffd0dc40
CC(C)(C)OC(=O)NCCOCCn1cnc2c[n+]([O-])c3ccccc3c21.[NH4+]>>CC(C)(C)OC(=O)NCCOCCn1cnc2c(N)nc3ccccc3c21
[NH4+].[OH-].[O-][N+]1=CC2=C(C=3C=CC=CC13)N(C=N2)CCOCCNC(OC(C)(C)C)=O.[NH4+].[OH-].C(Cl)Cl.C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>NC1=NC=2C=CC=CC2C2=C1N=CN2CCOCCNC(OC(C)(C)C)=O
[O-][n+:20]1[cH:18][c:17]2[n:16][cH:15][n:14]([CH2:13][CH2:12][O:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[c:27]2[c:26]2[c:21]1[cH:22][cH:23][cH:24][cH:25]2.[NH4+:19]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][n:14]1[cH:15][n:16][c:17]2[c...
CC(C)(C)OC(=O)NCCOCCn1cnc2c[n+]([O-])c3ccccc3c21.[NH4+]
CC(C)(C)OC(=O)NCCOCCn1cnc2c(N)nc3ccccc3c21
null
null
ClCCCl
Protection
OtherReaction
4cb72433be7a0d843d29843bff9411bfad039899e2cd9347e2313d8f7a557ce7
bf08eb59ebe808bce722373055de9689551bb60b2522898c82bc26646fc1fe40
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[n+;H0;D3:7](-[O-]):[c:8](:[c:9]):[c:10]:[c:11]:1:2.[NH4+;D0:12]>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:11]:1:[c:10]:[c:8](:[c:9]):[n;H0;D2;+0:7]:[c;H0;D3;+0:6]:2-[NH2;D1;+0:12]
null
[]
null
null
3
HOUR
A solution of tert-butyl 2-[2-(5-oxido-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (4.60 g, 12.4 mmol) in 150 mL of 1,2-dichloroethane was heated to 80° C. and treated with 10 mL of concentrated NH4OH solution. To the rapidly stirred solution was added solid p-toluenesulfonyl chloride (2.71 g, 14.2 mmol) over ...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1ccc2c(c1)[n+]cc1[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
c1nc2ccccc2c2[nH]cnc12
HO-
ClCCCl
null
3
CC(C)(C)OC(=O)NCCOCCn1cnc2c[n+]([O-])c3ccccc3c21.[NH4+]>ClCCCl>CC(C)(C)OC(=O)NCCOCCn1cnc2c(N)nc3ccccc3c21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1ce376451fa04f1bb3754c5fca6b00e9
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.COC(C)(OC)OC>>Cc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
Cl.[NH+]1=CC=CC=C1.NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O.C(C)(OC)(OC)OC>>CC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O
[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][O:17][CH2:18][CH2:19][NH:20][C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27].CO[C:2](OC)(OC)[CH3:1]>>[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][O:17][CH2:18]...
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.COC(C)(OC)OC
Cc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
ClCCCl
Aromatic Heterocycle Formation
OtherReaction
af7d6de7ca5153ecd31a13d7075f2969261301df4b656bfec36bc67fd1ea176b
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc2c(c1)ncc1nc[nH]c12
C-O-[C;H0;D4;+0:1](-[C;D1;H3:2])(-O-C)-O-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]
83.5
[{"value": 83.5, "product": "CC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (12.05 g, 34.8 mmol) in 200 mL of 1,2-dichloroethane was treated with trimethyl orthoacetate (5.50 mL, 43.2 mmol) and the reaction mixture was heated to reflux. A 100 mg portion of pyridinium hydrochloride was then added and refluxing was ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
ClCCCl
null
4
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.COC(C)(OC)OC>ClCCCl>Cc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9c2d1c90c4e84cef81a46bfd4a33ed83
Cc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C>>Cc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
CC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O.ClC=1C=C(C(=O)OO)C=CC1>>CC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O
[CH3:1][c:2]1[n:3][c:4]2[cH:5][n:6][c:8]3[cH:9][cH:10][cH:11][cH:12][c:13]3[c:14]2[n:15]1[CH2:16][CH2:17][O:18][CH2:19][CH2:20][NH:21][C:22](=[O:23])[O:24][C:25]([CH3:26])([CH3:27])[CH3:28]>>[CH3:1][c:2]1[n:3][c:4]2[cH:5][n+:6]([O-:7])[c:8]3[cH:9][cH:10][cH:11][cH:12][c:13]3[c:14]2[n:15]1[CH2:16][CH2:17][O:18][CH2:19][...
Cc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
Cc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)(Cl)Cl
Functional Group Interconversion
OtherReaction
d6328bcdf13aade6d233961c67aa0027be57934158b58a73811db431a33571a7
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
c1ccc2c(c1)[nH+]cc1nc[nH]c12
[c:1]:[c:2]1:[c:3]:[c:4]2:[#7;a:5]:[c:6]:[#7;a:7]:[c:8]:2:[c:9]:[n;H0;D2;+0:10]:1>>[O;-;D1;H0:11]-[n+;H0;D3:10]1:[c:9]:[c:8]2:[#7;a:7]:[c:6]:[#7;a:5]:[c:4]:2:[c:3]:[c:2]:1:[c:1]
100
[{"value": 100.0, "product": "CC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
A solution of tert-butyl 2-[2-(2-methyl-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (10.75 g, 29.0 mmol) in 150 mL of CHCl3 was chilled in an ice water bath. The solution was treated with 3-chloroperoxybenzoic acid (MCPBA, 70%, 10.73 g, 43.5 mmol). After stirring for 1.5 h, the reaction mixture was washed with...
10.6084/m9.figshare.5104873.v1
null
null
null
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(c[n+]c3ccccc32)[nH]1
null
C(Cl)(Cl)Cl
null
1.5
Cc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C>C(Cl)(Cl)Cl>Cc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ad22fad7618b47e8ab9aa84a2b90f1a4
Cc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>>Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
C1(=CC=C(C=C1)S(=O)(=O)Cl)C.O.CC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O.[NH4+].[OH-]>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(OC(C)(C)C)=O)C
[O-][n+:7]1[cH:5][c:4]2[n:3][c:2]([CH3:1])[n:15]([CH2:16][CH2:17][O:18][CH2:19][CH2:20][NH:21][C:22](=[O:23])[O:24][C:25]([CH3:26])([CH3:27])[CH3:28])[c:14]2[c:13]2[c:8]1[cH:9][cH:10][cH:11][cH:12]2.[NH4+:6]>>[CH3:1][c:2]1[n:3][c:4]2[c:5]([NH2:6])[n:7][c:8]3[cH:9][cH:10][cH:11][cH:12][c:13]3[c:14]2[n:15]1[CH2:16][CH2:1...
Cc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]
Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)Cl
Protection
OtherReaction
1a3560ac88422fd247b995f02bc4ff4290625edd39947787fab7dac607ad70df
bf08eb59ebe808bce722373055de9689551bb60b2522898c82bc26646fc1fe40
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[n+;H0;D3:7](-[O-]):[c:8](:[c:9]):[c:10]:[c:11]:1:2.[NH4+;D0:12]>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:11]:1:[c:10]:[c:8](:[c:9]):[n;H0;D2;+0:7]:[c;H0;D3;+0:6]:2-[NH2;D1;+0:12]
null
[]
null
null
null
null
A solution of tert-butyl 2-[2-(2-methyl-5-oxido-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (11.21 g, 29.0 mmol) in 75 mL of CH2Cl2 was treated with 75 mL of concentrated NH4OH solution. The mixture was chilled in an ice water bath. To the rapidly stirred mixture was added solid p-toluenesulfonyl chloride (5.5...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
C(Cl)Cl
null
null
Cc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>C(Cl)Cl>Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0569a42b9c0347a4bad5f00be9b86b7b
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCC(=O)Cl>>CCC(=O)Nc1cnc2ccccc2c1NCCOCCNC(=O)OC(C)(C)C
O.C(CC)(=O)Cl.NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O.C(C)N(CC)CC>>C(CC)(=O)NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O
[NH2:5][c:6]1[cH:7][n:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]2[c:15]1[NH:16][CH2:17][CH2:18][O:19][CH2:20][CH2:21][NH:22][C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29].Cl[C:3]([CH2:2][CH3:1])=[O:4]>>[CH3:1][CH2:2][C:3](=[O:4])[NH:5][c:6]1[cH:7][n:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]2[c:15]1[NH:16][CH2...
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCC(=O)Cl
CCC(=O)Nc1cnc2ccccc2c1NCCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc2ncccc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C;D1;H3:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]:[#7;a:9]:[c:10]>>[C;D1;H3:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]:[#7;a:9]:[c:10]
44.6
[{"value": 44.6, "product": "C(CC)(=O)NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (32.0 g, 92.0 mmol) in 300 mL of CH2Cl2 was treated with triethylamine (19.2 mL, 138.0 mmol). The reaction was chilled in an ice water bath and then propionyl chloride (9.40 mL, 108.2 mmol) was added dropwise. After stirring for 18 h, the ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2ncccc2c1
HCl
C(Cl)Cl
null
18
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCC(=O)Cl>C(Cl)Cl>CCC(=O)Nc1cnc2ccccc2c1NCCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-571380899b164b708bcd1efb417dc5c2
CCC(=O)Nc1cnc2ccccc2c1NCCOCCNC(=O)OC(C)(C)C>>CCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
C(CC)(=O)NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O.C(C)N(CC)CC>>C(C)C=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O
O=[C:3]([CH2:2][CH3:1])[NH:4][c:5]1[cH:6][n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[c:14]1[NH:15][CH2:16][CH2:17][O:18][CH2:19][CH2:20][NH:21][C:22](=[O:23])[O:24][C:25]([CH3:26])([CH3:27])[CH3:28]>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[cH:6][n:7][c:8]3[cH:9][cH:10][cH:11][cH:12][c:13]3[c:14]2[n:15]1[CH2:16][CH2:17][O:18]...
CCC(=O)Nc1cnc2ccccc2c1NCCOCCNC(=O)OC(C)(C)C
CCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
CCO
Aromatic Heterocycle Formation
OtherReaction
048882f89ec680a0d34f3902d9572ee75568aa993a5f9bf900f7615492f9fa85
71fdeda1d5481ba7466e825735d29b5ffca597c091e9548c43a80a0aea31b8a0
c1ccc2c(c1)ncc1nc[nH]c12
O=[C;H0;D3;+0:1](-[C:2]-[C;D1;H3:3])-[NH;D2;+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:13]-[C:12]-[n;H0;D3;+0:11]1:[c:10]2:[c:9]:[c:8]:[#7;a:7]:[c:6]:[c:5]:2:[n;H0;D2;+0:4]:[c;H0;D3;+0:1]:1-[C:2]-[C;D1;H3:3]
96.1
[{"value": 96.1, "product": "C(C)C=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
DAY
A solution of tert-butyl 2-(2-{[3-(propionylamino)quinolin-4-yl]amino}ethoxy)ethylcarbamate (15.00 g, 37.3 mmol) in 200 mL of EtOH was treated with triethylamine (13.0 mL, 93.2 mmol). The reaction was heated to reflux with stirring. After 3 days, the reaction was concentrated, triturated with ether and filtered to yiel...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
CCO
null
72
CCC(=O)Nc1cnc2ccccc2c1NCCOCCNC(=O)OC(C)(C)C>CCO>CCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-910b95784d7147cbbcbb86c388961372
CCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C>>CCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
O.C(C)C=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O.ClC=1C=C(C(=O)OO)C=CC1>>C(C)C=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O
[CH3:1][CH2:2][c:3]1[n:4][c:5]2[cH:6][n:7][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:16]1[CH2:17][CH2:18][O:19][CH2:20][CH2:21][NH:22][C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29]>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[cH:6][n+:7]([O-:8])[c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:16]1[CH2:17][CH2:18...
CCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
CCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)(Cl)Cl
Functional Group Interconversion
OtherReaction
d6328bcdf13aade6d233961c67aa0027be57934158b58a73811db431a33571a7
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
c1ccc2c(c1)[nH+]cc1nc[nH]c12
[c:1]:[c:2]1:[c:3]:[c:4]2:[#7;a:5]:[c:6]:[#7;a:7]:[c:8]:2:[c:9]:[n;H0;D2;+0:10]:1>>[O;-;D1;H0:11]-[n+;H0;D3:10]1:[c:9]:[c:8]2:[#7;a:7]:[c:6]:[#7;a:5]:[c:4]:2:[c:3]:[c:2]:1:[c:1]
100.1
[{"value": 100.1, "product": "C(C)C=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
A solution of tert-butyl 2-[2-(2-ethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (13.78 g 35.8 mmol) in 175 mL of CHCl3 was treated with 3-chloroperoxybenzoic acid (MCPBA, 70%, 10.28 g, 41.7 mmol). After stirring for 3 h, the reaction mixture was treated with water (100 mL) and CHCl3 (50 mL) and the layers w...
10.6084/m9.figshare.5104873.v1
null
null
null
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(c[n+]c3ccccc32)[nH]1
null
C(Cl)(Cl)Cl
null
3
CCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C>C(Cl)(Cl)Cl>CCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e3234ef3a01a4bbdb5857f11ce2d2695
CCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>>CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
C1(=CC=C(C=C1)S(=O)(=O)Cl)C.O.C(C)C=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O.[NH4+].[OH-]>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(OC(C)(C)C)=O)CC
[O-][n+:8]1[cH:6][c:5]2[n:4][c:3]([CH2:2][CH3:1])[n:16]([CH2:17][CH2:18][O:19][CH2:20][CH2:21][NH:22][C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29])[c:15]2[c:14]2[c:9]1[cH:10][cH:11][cH:12][cH:13]2.[NH4+:7]>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:16...
CCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]
CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)Cl
Protection
OtherReaction
1a3560ac88422fd247b995f02bc4ff4290625edd39947787fab7dac607ad70df
bf08eb59ebe808bce722373055de9689551bb60b2522898c82bc26646fc1fe40
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[n+;H0;D3:7](-[O-]):[c:8](:[c:9]):[c:10]:[c:11]:1:2.[NH4+;D0:12]>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:11]:1:[c:10]:[c:8](:[c:9]):[n;H0;D2;+0:7]:[c;H0;D3;+0:6]:2-[NH2;D1;+0:12]
null
[]
null
null
30
MINUTE
A solution of tert-butyl 2-[2-(2-ethyl-5-oxido-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (14.3 g, 35.8 mmol) in 90 mL of CH2Cl2 was treated with 90 mL of concentrated NH4OH solution. The mixture was chilled in an ice water bath. To the rapidly stirred mixture was added solid p-toluenesulfonyl chloride (7.05 ...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
C(Cl)Cl
null
0.5
CCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>C(Cl)Cl>CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-026743350d314774b776e8b50d32dafc
CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C>>CCc1nc2c(N)nc3ccccc3c2n1CCOCCN
NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(OC(C)(C)C)=O)CC>>NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)CC
CC(C)(C)OC(=O)[NH:22][CH2:21][CH2:20][O:19][CH2:18][CH2:17][n:16]1[c:3]([CH2:2][CH3:1])[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]21>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:16]1[CH2:17][CH2:18][O:19][CH2:20][CH2:21][NH2:22]
CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN
null
null
Cl.CCO
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2c(c1)ncc1nc[nH]c12
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
94.5
[{"value": 94.5, "product": "NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
Tert-butyl 2-[2-(4-amino-2-ethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate (9.35 g, 23.4 mmol) was suspended in 150 mL of 2M HCl in EtOH and the mixture was heated to reflux with stirring. After 2 h, the reaction was cooled to room temperature and the HCl salt of the product was collected by vacuum filtratio...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1nc2c(cnc3ccccc32)[nH]1
HO-
Cl.CCO
null
2
CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C>Cl.CCO>CCc1nc2c(N)nc3ccccc3c2n1CCOCCN
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5961be4f5d6142b394967d6ed4ff22aa
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCOCC(=O)Cl>>CCOCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
NC=1C=NC2=CC=CC=C2C1NCCOCCNC(OC(C)(C)C)=O.C(C)OCC(=O)Cl>>C(C)OCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O
[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1[NH:17][CH2:18][CH2:19][O:20][CH2:21][CH2:22][NH:23][C:24](=[O:25])[O:26][C:27]([CH3:28])([CH3:29])[CH3:30].O=[C:5](Cl)[CH2:4][O:3][CH2:2][CH3:1]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][cH:12][cH:13][cH:14][c:15]3[c:1...
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCOCC(=O)Cl
CCOCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
CN(C1=CC=NC=C1)C
N1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
2849961f1d737a23d71906fe74b0976730547255ac052bf4a7367ba2be72dd8e
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[#8:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[#8:3]-[C:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:13]:[c:12]2:[c:11]:[#7;a:10]:[c:9]:[c:8]:[c:7]:2:[n;H0;D3;+0:6]:1-[C:5]-[C:4]
71.6
[{"value": 71.6, "product": "C(C)OCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (18.04 g, 52.1 mmol) in 180 mL of pyridine was treated with 50 mg of 4-dimethylaminopyridine and chilled in an ice water bath. 2-ethoxyacetyl chloride (6.44 g, 52.6 mmol) was added dropwise to the solution. The reaction was stirred at room...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HCl
CN(C1=CC=NC=C1)C.N1=CC=CC=C1
null
3
CC(C)(C)OC(=O)NCCOCCNc1c(N)cnc2ccccc12.CCOCC(=O)Cl>CN(C1=CC=NC=C1)C.N1=CC=CC=C1>CCOCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-07073e660b9b4e25bfb17ed15f86f7c0
CCOCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1>>CCOCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
O.C(C)OCC=1N(C2=C(C=NC=3C=CC=CC23)N1)CCOCCNC(OC(C)(C)C)=O.ClC=1C=C(C(=O)OO)C=CC1>>C(C)OCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O
[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31].O=C(O[OH:10])c1cccc(Cl)c1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n+:9]([O-:10])[c:11]3[cH:12][cH:...
CCOCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1
CCOCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)(Cl)Cl
Miscellaneous
OtherReaction
86abb75bf448eea8ddd78de30fcfc7b06bb61e46f725af6f1625e0dd9537993c
98b338a9d01476c0929fd5672e7509121bfe69600fd72e4d1cc6f1782e2d05d9
c1ccc2c(c1)[nH+]cc1nc[nH]c12
Cl-c1:c:c:c:c(-C(=O)-O-[OH;D1;+0:1]):c: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]
100
[{"value": 100.0, "product": "C(C)OCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
A solution of tert-butyl 2-{2-[2-(ethoxymethyl)-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethylcarbamate (15.47 g, 37.3 mmol) in 150 mL of CHCl3 was treated with 3-chloroperoxybenzoic acid (MCPBA, 70%, 15.12 g, 61.3 mmol). After stirring for 1.5 h, the reaction mixture was treated with water (100 mL) and CHCl3 (50 mL) and ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Peroxide
null
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(c[n+]c3ccccc32)[nH]1
HCl
C(Cl)(Cl)Cl
null
1.5
CCOCc1nc2cnc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.O=C(OO)c1cccc(Cl)c1>C(Cl)(Cl)Cl>CCOCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-12ef87c0fecb4344b0ed4f6da7392c8a
CCOCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
C1(=CC=C(C=C1)S(=O)(=O)Cl)C.O.C(C)OCC=1N(C2=C(C=[N+](C=3C=CC=CC23)[O-])N1)CCOCCNC(OC(C)(C)C)=O.[NH4+].[OH-]>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(OC(C)(C)C)=O)COCC
[O-][n+:10]1[cH:8][c:7]2[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:18]([CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31])[c:17]2[c:16]2[c:11]1[cH:12][cH:13][cH:14][cH:15]2.[NH4+:9]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:1...
CCOCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
null
null
C(Cl)Cl
Protection
OtherReaction
1a3560ac88422fd247b995f02bc4ff4290625edd39947787fab7dac607ad70df
bf08eb59ebe808bce722373055de9689551bb60b2522898c82bc26646fc1fe40
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[n+;H0;D3:7](-[O-]):[c:8](:[c:9]):[c:10]:[c:11]:1:2.[NH4+;D0:12]>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:11]:1:[c:10]:[c:8](:[c:9]):[n;H0;D2;+0:7]:[c;H0;D3;+0:6]:2-[NH2;D1;+0:12]
null
[]
null
null
30
MINUTE
A solution of tert-butyl 2-{2-[2-(ethoxymethyl)-5-oxido-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethylcarbamate (16.06 g, 37.3 mmol) in 75 mL of CH2Cl2 was treated with 75 mL of concentrated NH4OH solution. The mixture was chilled in an ice water bath. To the rapidly stirred mixture was added solid p-toluenesulfonyl chlor...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1nc2c(c[n+]c3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HO-
C(Cl)Cl
null
0.5
CCOCc1nc2c[n+]([O-])c3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C.[NH4+]>C(Cl)Cl>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-07358473e4244b4fbb6a1a0e0af73249
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C>>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN
NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(OC(C)(C)C)=O)COCC.CCOCC.C>>NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)COCC
CC(C)(C)OC(=O)[NH:24][CH2:23][CH2:22][O:21][CH2:20][CH2:19][n:18]1[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]21>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:...
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN
null
null
Cl.CCO.CO
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2c(c1)ncc1nc[nH]c12
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
null
null
3
HOUR
Tert-butyl 2-{2-[4-amino-2-(ethoxymethyl)-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethylcarbamate (14.45 g, 33.6 mmol) was dissolved in 50 mL of 2M HCl in EtOH and the mixture was heated to reflux with stirring. After 3 h, the reaction was cooled to room temperature and treated with ether (100 mL). The HCl salt of the pro...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1nc2c(cnc3ccccc32)[nH]1
HO-
Cl.CCO.CO
null
3
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)OC(C)(C)C>Cl.CCO.CO>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3571e8c7e7a2428fb31e2a319cae278e
Cc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1>>Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
C1(=CC=CC=C1)N=C=O.NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)C.C(C)N(CC)CC>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)C
[CH3:1][c:2]1[n:3][c:4]2[c:5]([NH2:6])[n:7][c:8]3[cH:9][cH:10][cH:11][cH:12][c:13]3[c:14]2[n:15]1[CH2:16][CH2:17][O:18][CH2:19][CH2:20][NH2:21].[C:22](=[O:23])=[N:24][c:25]1[cH:26][cH:27][cH:28][cH:29][cH:30]1>>[CH3:1][c:2]1[n:3][c:4]2[c:5]([NH2:6])[n:7][c:8]3[cH:9][cH:10][cH:11][cH:12][c:13]3[c:14]2[n:15]1[CH2:16][CH2...
Cc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1
Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
null
null
CN1C(CCC1)=O
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCOCCn1cnc2cnc3ccccc3c21)Nc1ccccc1
[C:1]-[C:2]-[NH2;D1;+0:3].[O;D1;H0:4]=[C;H0;D2;+0:5]=[N;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:5](=[O;D1;H0:4])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]
17.5
[{"value": 17.5, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of the compound of Example 45, 1-[2-(2-aminoethoxy)ethyl]-2-methyl-1H-imidazo[4,5-c]quinolin-4-amine (1.411 g, 4.95 mmol) in 40 mL of 1-methyl-2-pyrrolidinone was treated with triethylamine (1.38 mL, 9.89 mmol). With vigorous stirring, the solution was treated with phenyl isocyanate (0.538, 4.95 mmol). After...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
null
CN1C(CCC1)=O
null
18
Cc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1>CN1C(CCC1)=O>Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d10c0e9f152c48619e590ba05d36faf3
Cc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1>>Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)C.C1(CCCCC1)N=C=O>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2CCCCC2)C
[CH3:1][c:2]1[n:3][c:4]2[c:5]([NH2:6])[n:7][c:8]3[cH:9][cH:10][cH:11][cH:12][c:13]3[c:14]2[n:15]1[CH2:16][CH2:17][O:18][CH2:19][CH2:20][NH2:21].[C:22](=[O:23])=[N:24][CH:25]1[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]1>>[CH3:1][c:2]1[n:3][c:4]2[c:5]([NH2:6])[n:7][c:8]3[cH:9][cH:10][cH:11][cH:12][c:13]3[c:14]2[n:15]1[CH2:1...
Cc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1
Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
null
null
N1=CC=CC=C1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCOCCn1cnc2cnc3ccccc3c21)NC1CCCCC1
[C:1]-[C:2](-[N;H0;D2;+0:3]=[C;H0;D2;+0:4]=[O;D1;H0:5])-[C:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[NH;D2;+0:3]-[C:2](-[C:1])-[C:6]
49.8
[{"value": 49.8, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2CCCCC2)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of the compound of Example 45, 1-[2-(2-aminoethoxy)ethyl]-2-methyl-1H-imidazo[4,5-c]quinolin-4-amine (1.00 g, 3.50 mmol) in 30 mL of pyridine was chilled in an ice water bath. With vigorous stirring, the solution was treated with cyclohexyl isocyanate (0.45 mL, 3.50 mmol). After 18 h, the reaction was concen...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.C1CCCCC1
null
N1=CC=CC=C1
null
18
Cc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1>N1=CC=CC=C1>Cc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f7c8e7283245442d9576f577b680b160
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1>>CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)CC.C1(=CC=CC=C1)N=C=O>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)CC
[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:16]1[CH2:17][CH2:18][O:19][CH2:20][CH2:21][NH2:22].[C:23](=[O:24])=[N:25][c:26]1[cH:27][cH:28][cH:29][cH:30][cH:31]1>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:...
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1
CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
null
null
C(Cl)Cl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCOCCn1cnc2cnc3ccccc3c21)Nc1ccccc1
[C:1]-[C:2]-[NH2;D1;+0:3].[O;D1;H0:4]=[C;H0;D2;+0:5]=[N;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:5](=[O;D1;H0:4])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]
50
[{"value": 50.0, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of the compound of Example 46, 1-[2-(2-aminoethoxy)ethyl]-2-ethyl-1H-imidazo[4,5-c]quinolin-4-amine (800 mg, 2.67 mmol) in 30 mL of CH2Cl2 was stirred vigorously and treated with phenyl isocyanate (0.290 mL, 2.67 mmol). After 18 h, the reaction was concentrated to yield an off white solid. Purification by co...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
null
C(Cl)Cl
null
18
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1>C(Cl)Cl>CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3fb82c96c7c047cb97bf2aef937dc8db
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1>>CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)CC.C1(CCCCC1)N=C=O>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2CCCCC2)CC
[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:16]1[CH2:17][CH2:18][O:19][CH2:20][CH2:21][NH2:22].[C:23](=[O:24])=[N:25][CH:26]1[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]1>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:1...
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1
CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
null
null
N1=CC=CC=C1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCOCCn1cnc2cnc3ccccc3c21)NC1CCCCC1
[C:1]-[C:2](-[N;H0;D2;+0:3]=[C;H0;D2;+0:4]=[O;D1;H0:5])-[C:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[NH;D2;+0:3]-[C:2](-[C:1])-[C:6]
66
[{"value": 66.0, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2CCCCC2)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A solution of the compound of Example 46, 1-[2-(2-aminoethoxy)ethyl]-2-ethyl-1H-imidazo[4,5-c]quinolin-4-amine (800 mg, 2.67 mmol) in 30 mL of pyridine was chilled in an ice water bath. With vigorous stirring, the solution was treated with cyclohexyl isocyanate (0.340 mL, 2.67 mmol). After 1 h, the reaction was concent...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.C1CCCCC1
null
N1=CC=CC=C1
null
1
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1>N1=CC=CC=C1>CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bcd118c363164abaab40fe2ee9cec2d2
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1>>CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)CC.N1(CCOCC1)C(=O)Cl>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)N2CCOCC2)CC
[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:16]1[CH2:17][CH2:18][O:19][CH2:20][CH2:21][NH2:22].Cl[C:23](=[O:24])[N:25]1[CH2:26][CH2:27][O:28][CH2:29][CH2:30]1>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2[n:16...
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1
CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
null
null
N1=CC=CC=C1
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
b81fefae7607aa106605114867756af2924064950a2aea97200543849613e96a
406c5893488430105533c87dfb5d625d8382e709e047cda9cfdc2235e742a9cf
O=C(NCCOCCn1cnc2cnc3ccccc3c21)N1CCOCC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C:4])-[C:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C:4])-[C:5]
51.1
[{"value": 51.1, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)N2CCOCC2)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A solution of the compound of Example 46, 1-[2-(2-aminoethoxy)ethyl]-2-ethyl-1H-imidazo[4,5-c]quinolin-4-amine (800 mg, 2.67 mmol) in 30 mL of pyridine was chilled in an ice water bath. With vigorous stirring, the solution was treated with 4-morpholinecarbonyl chloride (0.310 mL, 2.67 mmol). After 1 h, the reaction was...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Tertiary amide.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.C1COCC[NH]1
HCl
N1=CC=CC=C1
null
1
CCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1>N1=CC=CC=C1>CCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1625d23f71b84467a4005b078878a38c
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1>>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)COCC.C1(=CC=CC=C1)N=C=O>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)COCC
[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH2:24].[C:25](=[O:26])=[N:27][c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH...
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
null
null
C(Cl)Cl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCOCCn1cnc2cnc3ccccc3c21)Nc1ccccc1
[C:1]-[C:2]-[NH2;D1;+0:3].[O;D1;H0:4]=[C;H0;D2;+0:5]=[N;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:5](=[O;D1;H0:4])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]
39.6
[{"value": 39.6, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2=CC=CC=C2)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A solution of the compound of Example 47, 1-[2-(2-aminoethoxy)ethyl]-2-(ethoxymethyl)-1H-imidazo[4,5-c]quinolin-4-amine (980 mg, 2.98 mmol) in 20 mL of CH2Cl2 was chilled in an ice water bath. With vigorous stirring, the solution was treated with phenyl isocyanate (0.340 mL, 3.13 mmol). After 30 min, the reaction was c...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.c1ccccc1
null
C(Cl)Cl
null
0.5
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=Nc1ccccc1>C(Cl)Cl>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)Nc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-806811f7f51242b38aae9480947e1d1d
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1>>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)COCC.C1(CCCCC1)N=C=O>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2CCCCC2)COCC
[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH2:24].[C:25](=[O:26])=[N:27][CH:28]1[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:...
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
null
null
C(Cl)Cl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCOCCn1cnc2cnc3ccccc3c21)NC1CCCCC1
[C:1]-[C:2](-[N;H0;D2;+0:3]=[C;H0;D2;+0:4]=[O;D1;H0:5])-[C:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[NH;D2;+0:3]-[C:2](-[C:1])-[C:6]
29.5
[{"value": 29.5, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)NC2CCCCC2)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A solution of the compound of Example 47, 1-[2-(2-aminoethoxy)ethyl]-2-(ethoxymethyl)-1H-imidazo[4,5-c]quinolin-4-amine (980 mg, 2.98 mmol) in 20 mL of CH2Cl2 was chilled in an ice water bath. With vigorous stirring, the solution was treated with cyclohexyl isocyanate (0.400 mL, 3.13 mmol). After 30 min, the reaction w...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.C1CCCCC1
null
C(Cl)Cl
null
0.5
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C=NC1CCCCC1>C(Cl)Cl>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)NC1CCCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-398d20b3e2494afbae52c5075d30027e
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1>>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
N1(CCOCC1)C(=O)Cl.O.NCCOCCN1C(=NC=2C(=NC=3C=CC=CC3C21)N)COCC.C(C)N(CC)CC>>NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)N2CCOCC2)COCC
[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][O:21][CH2:22][CH2:23][NH2:24].Cl[C:25](=[O:26])[N:27]1[CH2:28][CH2:29][O:30][CH2:31][CH2:32]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][cH:13][cH:1...
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
null
null
C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
b81fefae7607aa106605114867756af2924064950a2aea97200543849613e96a
406c5893488430105533c87dfb5d625d8382e709e047cda9cfdc2235e742a9cf
O=C(NCCOCCn1cnc2cnc3ccccc3c21)N1CCOCC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C:4])-[C:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C:4])-[C:5]
29.8
[{"value": 29.8, "product": "NC1=NC=2C=CC=CC2C2=C1N=C(N2CCOCCNC(=O)N2CCOCC2)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of the compound of Example 47, 1-[2-(2-aminoethoxy)ethyl]-2-(ethoxymethyl)-1H-imidazo[4,5-c]quinolin-4-amine (980 mg, 2.98 mmol) in 20 mL of CH2Cl2 was treated with triethylamine (1.04 mL, 7.45 mmol) and chilled in an ice water bath. With vigorous stirring, the solution was treated with 4-morpholinecarbonyl ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Tertiary amide.Primary amine
Urea
null
null
c1nc2c(cnc3ccccc32)[nH]1.C1COCC[NH]1
HCl
C(Cl)Cl
null
18
CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCN.O=C(Cl)N1CCOCC1>C(Cl)Cl>CCOCc1nc2c(N)nc3ccccc3c2n1CCOCCNC(=O)N1CCOCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6ab0c792e2884cc19df6d6ecb4a193da
CC1(C)CN=C(Cc2ccccc2)C1.O=C(CBr)c1ccc(Cl)cc1>>CC1(C)Cc2c(-c3ccccc3)c(-c3ccc(Cl)cc3)cn2C1
C1=CC(=CC=C1C(=O)CBr)Cl.C(C1=CC=CC=C1)C1=NCC(C1)(C)C>>ClC1=CC=C(C=C1)C1=CN2CC(CC2=C1C1=CC=CC=C1)(C)C
[CH3:1][C:2]1([CH3:3])[CH2:4][C:5]([CH2:6][c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)=[N:22][CH2:23]1.O=[C:13]([c:14]1[cH:15][cH:16][c:17]([Cl:18])[cH:19][cH:20]1)[CH2:21]Br>>[CH3:1][C:2]1([CH3:3])[CH2:4][c:5]2[c:6](-[c:7]3[cH:8][cH:9][cH:10][cH:11][cH:12]3)[c:13](-[c:14]3[cH:15][cH:16][c:17]([Cl:18])[cH:19][cH:20]3)[cH:...
CC1(C)CN=C(Cc2ccccc2)C1.O=C(CBr)c1ccc(Cl)cc1
CC1(C)Cc2c(-c3ccccc3)c(-c3ccc(Cl)cc3)cn2C1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b6a3fcda43f0dc538a3fb7598130630c97a7f6c654ec5e8d741fa2c8fffe2c2c
5d16d986f2820f4a8c80dd26fbdf56b0677fe2763d9991e54a666fed55014ae0
c1ccc(-c2cn3c(c2-c2ccccc2)CCC3)cc1
Br-[CH2;D2;+0:1]-[C;H0;D3;+0:2](=O)-[c;H0;D3;+0:3](:[c:4]:[c:5]):[c:6]:[c:7].[c:8]:[c:9]:[c;H0;D3;+0:10](-[CH2;D2;+0:11]-[C;H0;D3;+0:12]1=[N;H0;D2;+0:13]-[C:14]-[C:15]-[C:16]-1):[c:17]:[c:18]>>[c:8]:[c:9]:[c;H0;D3;+0:10](-[c;H0;D3;+0:11]1:[c;H0;D3;+0:2](-[c;H0;D3;+0:3](:[c:4]:[c:5]):[c:6]:[c:7]):[cH;D2;+0:1]:[n;H0;D3;+...
null
[]
null
null
null
null
The 2-benzyl-4,4-dimethyl-1-pyrroline of the formula III is then cyclized with ω-bromo-4-chloroacetophenone to give the 6-(4-chlorophenyl)-2,2-dimethyl-7-phenyl-2,3-dihydro-1H-pyrrolizine of the formula II. The reaction is known from the prior art mentioned at the outset. ω-Bromo-4-chloroacetophenone can be obtained, f...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Substituted imine
null
C1=NCCC1
c1cc2n(c1)CCC2
c1ccccc1.c1ccccc1.c1cc2n(c1)CCC2
HBr
null
null
null
CC1(C)CN=C(Cc2ccccc2)C1.O=C(CBr)c1ccc(Cl)cc1>>CC1(C)Cc2c(-c3ccccc3)c(-c3ccc(Cl)cc3)cn2C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-238fae4e2e3046a0a1712d0feaaffa42
Cn1cccc1.O=C(Cl)C(Cl)(Cl)Cl>>O=C(c1ccc[nH]1)C(Cl)(Cl)Cl
ClC(C(=O)Cl)(Cl)Cl.CN1C=CC=C1>>ClC(C(=O)C=1NC=CC1)(Cl)Cl
C[n:7]1[cH:3][cH:4][cH:5][cH:6]1.Cl[C:2](=[O:1])[C:8]([Cl:9])([Cl:10])[Cl:11]>>[O:1]=[C:2]([c:3]1[cH:4][cH:5][cH:6][nH:7]1)[C:8]([Cl:9])([Cl:10])[Cl:11]
Cn1cccc1.O=C(Cl)C(Cl)(Cl)Cl
O=C(c1ccc[nH]1)C(Cl)(Cl)Cl
null
null
C(C)OCC
C-C Coupling
OtherReaction
701d21b652ce6d90463464dd21d4d87caf603bff2f60e1ad8fa59cfd59145f4f
fe2a4a0dfbb5b71b9a065e092364c64b22b4eb1ad4d6ba2a1e8edc9d31fce3e4
c1cc[nH]c1
C-[n;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[cH;D2;+0:5]:1.Cl-[C;H0;D3;+0:6](=[O;D1;H0:7])-[C:8](-[Cl;D1;H0:9])(-[Cl;D1;H0:10])-[Cl;D1;H0:11]>>[Cl;D1;H0:9]-[C:8](-[Cl;D1;H0:10])(-[Cl;D1;H0:11])-[C;H0;D3;+0:6](=[O;D1;H0:7])-[c;H0;D3;+0:5]1:[c:4]:[c:3]:[c:2]:[nH;D2;+0:1]:1
92.7
[{"value": 92.7, "product": "ClC(C(=O)C=1NC=CC1)(Cl)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a well stirred solution of trichloroacetyl chloride (1 kg, 5.5 mole) in 1.5 liter ethyl ether in a 12 liter flask was added dropwise over a period of 3 h a solution of N-methylpyrrole (0.45 kg, 5.5 mole) in 1.5 liter anhydrous ethyl ether. The reaction was stirred for an additional 3 hours and quenched by the dropwi...
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Ketone
c1cc[nH]c1
c1cc[nH]c1
c1cc[nH]c1
HCl
C(C)OCC
null
3
Cn1cccc1.O=C(Cl)C(Cl)(Cl)Cl>C(C)OCC>O=C(c1ccc[nH]1)C(Cl)(Cl)Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8051ad50dff14c47a524be7692963636
O=C(c1ccc[nH]1)C(Cl)(Cl)Cl.O=[N+]([O-])O>>Cn1cc([N+](=O)[O-])cc1C(=O)C(Cl)(Cl)Cl
ClC(C(=O)C=1NC=CC1)(Cl)Cl.[N+](=O)(O)[O-].C(C)(C)O>>[N+](=O)([O-])C=1C=C(N(C1)C)C(C(Cl)(Cl)Cl)=O
[nH:2]1[cH:3][cH:4][cH:8][c:9]1[C:10](=[O:11])[C:12]([Cl:13])([Cl:14])[Cl:15].O[N+:5](=[O:6])[O-:7]>>[CH3:1][n:2]1[cH:3][c:4]([N+:5](=[O:6])[O-:7])[cH:8][c:9]1[C:10](=[O:11])[C:12]([Cl:13])([Cl:14])[Cl:15]
O=C(c1ccc[nH]1)C(Cl)(Cl)Cl.O=[N+]([O-])O
Cn1cc([N+](=O)[O-])cc1C(=O)C(Cl)(Cl)Cl
null
null
C(C)(=O)OC(C)=O
Functional Group Addition
OtherReaction
30eec259f0a5a093f09ad410d85904ad6868c9951a256c4a4c8946d22adaf24a
ddce49825c02b8965f10c8d99e3c841d26e1f136da6037b417c09313e6d73097
c1cc[nH]c1
O-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3].[C:4]-[C:5](=[O;D1;H0:6])-[c:7]1:[c:8]:[cH;D2;+0:9]:[c:10]:[nH;D2;+0:11]:1>>[C:4]-[C:5](=[O;D1;H0:6])-[c:7]1:[c:8]:[c;H0;D3;+0:9](-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3]):[c:10]:[n;H0;D3;+0:11]:1-[C;D1;H3:12]
54
[{"value": 54.0, "product": "[N+](=O)([O-])C=1C=C(N(C1)C)C(C(Cl)(Cl)Cl)=O", "details": "PERCENTYIELD", "is_desired": false}]
-40
CELSIUS
4
HOUR
To a well stirred solution of trichloroacetyl chloride (1 kg, 5.5 mole) in 1.5 liter ethyl ether in a 12 liter flask was added dropwise over a period of 3 h a solution of N-methylpyrrole (0.45 kg, 5.5 mole) in 1.5 liter anhydrous ethyl ether. The reaction was stirred for an additional 3 hours and quenched by the dropwi...
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group
c1cc[nH]c1
c1cc[nH]c1
c1cc[nH]c1
null
C(C)(=O)OC(C)=O
-40
4
O=C(c1ccc[nH]1)C(Cl)(Cl)Cl.O=[N+]([O-])O>C(C)(=O)OC(C)=O>Cn1cc([N+](=O)[O-])cc1C(=O)C(Cl)(Cl)Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b9585db531774ec3bb0a2d3c2eeb1d60
c1ccc(P(c2ccccc2)c2ccccc2)cc1>>O=P(c1ccccc1)(c1ccccc1)c1ccccc1
CO.C(C)(C)(C)OC(=O)N([C@@H](C)CO)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.BrN1C(CCC1=O)=O>>C1(=CC=CC=C1)P(C1=CC=CC=C1)(C1=CC=CC=C1)=O
[P:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1)([c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)[c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1>>[O:1]=[P:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1)([c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)[c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1
c1ccc(P(c2ccccc2)c2ccccc2)cc1
O=P(c1ccccc1)(c1ccccc1)c1ccccc1
null
null
CN(C)C=O
Functional Group Interconversion
OtherReaction
42af6cdfb86a130c92365e01a31b50705eea7bdf12f67dc370bf24402f7ceedc
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
O=P(c1ccccc1)(c1ccccc1)c1ccccc1
[c:1]:[c:2](-[P;H0;D3;+0:3](-[c:4](:[c:5]):[c:6])-[c:7](:[c:8]):[c:9]):[c:10]>>[O;D1;H0:11]=[P;H0;D4;+0:3](-[c:4](:[c:5]):[c:6])(-[c:7](:[c:8]):[c:9])-[c:2](:[c:1]):[c:10]
85
[{"value": 85.0, "product": "C1(=CC=CC=C1)P(C1=CC=CC=C1)(C1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
To a solution of the N-tert-butoxycarbonyl phenyl alaninol (1.42 mmol) and triphenylphosphine (2 equiv) in DMF, N-bromosuccinimide (2 equiv) was slowly added. The reaction was warmed to 50° for 15 min and then cooled to 20°. Methanol (0.5 mL) was added to destroy the excess reagent. After 5 min, ether was added, and th...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1ccccc1.c1ccccc1
null
CN(C)C=O
null
0.083333
c1ccc(P(c2ccccc2)c2ccccc2)cc1>CN(C)C=O>O=P(c1ccccc1)(c1ccccc1)c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ad1da34fdff74ffd8ff1cfc5f671ee2b
C1CCNCC1.CC(C)(C)OC(=O)NC(CCBr)c1ccccc1>>NC(CCN1CCCCC1)c1ccccc1
BrCCC(C1=CC=CC=C1)NC(=O)OC(C)(C)C.N1CCCCC1>>C1(=CC=CC=C1)C(CCN1CCCCC1)N
[NH:5]1[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10]1.CC(C)(C)OC(=O)[NH:1][CH:2]([CH2:3][CH2:4]Br)[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[NH2:1][CH:2]([CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10]1)[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
C1CCNCC1.CC(C)(C)OC(=O)NC(CCBr)c1ccccc1
NC(CCN1CCCCC1)c1ccccc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
dbf8b9a06030f8030bf063f09fd042d89443a731c7712f62eb044a59b8cc9903
7617c42d56b550b3d1d0d0991f3f1bb85834fe99753d336fc35a923b06f52463
c1ccc(CCCN2CCCCC2)cc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3](-[c:4])-[NH;D2;+0:5]-C(=O)-O-C(-C)(-C)-C.[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3](-[NH2;D1;+0:5])-[c:4])-[C:9]-[C:10]
null
[]
null
null
null
null
The procedure given in Example 2 except for the formation of salts was followed using 3-bromo-1-(tert-butoxycarbonyl)amino-1-phenyl propane and piperidine as reactants, instead of d-1-bromo-2-(tert-butoxycarbonyl)amino-3-phenyl propane and hexamethyleneimine to give 1-Phenyl-3-(1-piperidinyl)-n-propylamine. Conditions:...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carbamic ester.Ether.Secondary amine.Boc
Primary amine.Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccccc1
HBr
null
null
null
C1CCNCC1.CC(C)(C)OC(=O)NC(CCBr)c1ccccc1>>NC(CCN1CCCCC1)c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-acd83b19b47d45b8a4f04bb5230bd5a2
CC(C)(C)OC(=O)NC(CCBr)c1ccccc1.OC(c1ccccc1)C1CCNCC1>>NC(CCN1CCC(C(O)c2ccccc2)CC1)c1ccccc1
BrCCC(C1=CC=CC=C1)NC(=O)OC(C)(C)C.C1(=CC=CC=C1)C(O)C1CCNCC1>>NC(CCN1CCC(CC1)C(O)C1=CC=CC=C1)C1=CC=CC=C1
CC(C)(C)OC(=O)[NH:1][CH:2]([CH2:3][CH2:4]Br)[c:19]1[cH:20][cH:21][cH:22][cH:23][cH:24]1.[NH:5]1[CH2:6][CH2:7][CH:8]([CH:9]([OH:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[CH2:17][CH2:18]1>>[NH2:1][CH:2]([CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][CH:8]([CH:9]([OH:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[CH2:17][CH2...
CC(C)(C)OC(=O)NC(CCBr)c1ccccc1.OC(c1ccccc1)C1CCNCC1
NC(CCN1CCC(C(O)c2ccccc2)CC1)c1ccccc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
dbf8b9a06030f8030bf063f09fd042d89443a731c7712f62eb044a59b8cc9903
7617c42d56b550b3d1d0d0991f3f1bb85834fe99753d336fc35a923b06f52463
c1ccc(CCCN2CCC(Cc3ccccc3)CC2)cc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3](-[c:4])-[NH;D2;+0:5]-C(=O)-O-C(-C)(-C)-C.[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3](-[NH2;D1;+0:5])-[c:4])-[C:9]-[C:10]
null
[]
null
null
null
null
The procedure given in Example 2 except for the formation of salts was followed using 3-bromo-1-(tert-butoxycarbonyl)amino-1-phenyl propane and phenyl-piperidin-4-yl-methanol as reactants, instead of d-1-bromo-2-(tert-butoxycarbonyl)amino-3-phenyl propane and hexamethyleneimine to give [1-(3-Amino-3-phenyl-propyl)-pipe...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carbamic ester.Ether.Secondary amine.Boc
Primary amine.Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccccc1.c1ccccc1
HBr
null
null
null
CC(C)(C)OC(=O)NC(CCBr)c1ccccc1.OC(c1ccccc1)C1CCNCC1>>NC(CCN1CCC(C(O)c2ccccc2)CC1)c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-00b0281c50da4bacb5aa3150161bb91c
CC(C)(C)OC(=O)NC(CCBr)c1ccccc1.OC(c1ccc(F)cc1)C1CCNCC1>>NC(CCN1CCC(C(O)c2ccc(F)cc2)CC1)c1ccccc1
BrCCC(C1=CC=CC=C1)NC(=O)OC(C)(C)C.FC1=CC=C(C=C1)C(O)C1CCNCC1>>NC(CCN1CCC(CC1)C(O)C1=CC=C(C=C1)F)C1=CC=CC=C1
CC(C)(C)OC(=O)[NH:1][CH:2]([CH2:3][CH2:4]Br)[c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1.[NH:5]1[CH2:6][CH2:7][CH:8]([CH:9]([OH:10])[c:11]2[cH:12][cH:13][c:14]([F:15])[cH:16][cH:17]2)[CH2:18][CH2:19]1>>[NH2:1][CH:2]([CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][CH:8]([CH:9]([OH:10])[c:11]2[cH:12][cH:13][c:14]([F:15])[cH:16][cH:17]...
CC(C)(C)OC(=O)NC(CCBr)c1ccccc1.OC(c1ccc(F)cc1)C1CCNCC1
NC(CCN1CCC(C(O)c2ccc(F)cc2)CC1)c1ccccc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
dbf8b9a06030f8030bf063f09fd042d89443a731c7712f62eb044a59b8cc9903
7617c42d56b550b3d1d0d0991f3f1bb85834fe99753d336fc35a923b06f52463
c1ccc(CCCN2CCC(Cc3ccccc3)CC2)cc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3](-[c:4])-[NH;D2;+0:5]-C(=O)-O-C(-C)(-C)-C.[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3](-[NH2;D1;+0:5])-[c:4])-[C:9]-[C:10]
null
[]
null
null
null
null
The procedure given in Example 2 was followed using 3-bromo-1-(tert-butoxycarbonyl)amino-1-phenyl propane and (4-fluorophenyl)-piperidin-4-yl-methanol as reactants, instead of d-1-bromo-2-(tert-butoxycarbonyl)amino-3-phenyl propane and hexamethyleneimine to give [1-(3-Amino-3-phenyl-propyl)-piperidin-4-yl]-(4-fluoro-ph...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carbamic ester.Ether.Secondary amine.Boc
Primary amine.Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccccc1.c1ccccc1
HBr
null
null
null
CC(C)(C)OC(=O)NC(CCBr)c1ccccc1.OC(c1ccc(F)cc1)C1CCNCC1>>NC(CCN1CCC(C(O)c2ccc(F)cc2)CC1)c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d519d927b6524e8eba036b10bc73760b
NC1CCC1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1>>O=[N+]([O-])c1cn(C2CCC2)cn1
[N+](=O)([O-])N1C=NC(=C1)[N+](=O)[O-].C1(CCC1)N>>C1(CCC1)N1C=NC(=C1)[N+](=O)[O-]
N[CH:7]1[CH2:8][CH2:9][CH2:10]1.O=[N+]([O-])[n:6]1[cH:5][c:4]([N+:2](=[O:1])[O-:3])[n:12][cH:11]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6]([CH:7]2[CH2:8][CH2:9][CH2:10]2)[cH:11][n:12]1
NC1CCC1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1
O=[N+]([O-])c1cn(C2CCC2)cn1
null
null
CO
Functional Group Addition
OtherReaction
46a51f8ca5a006fa0c7307aff9c47bbfab60ab29424e07318a72cc160ef81c35
e44bfec7c64c2106b9732634e34828e6460a6db63dcf75ef4a78a1aabdfc680a
c1cn(C2CCC2)cn1
N-[CH;D3;+0:1]1-[C:2]-[C:3]-[C:4]-1.O=[N+](-[O-])-[n;H0;D3;+0:5]1:[c:6]:[#7;a:7]:[c:8](-[#7;+:9]):[c:10]:1>>[#7;+:9]-[c:8]1:[#7;a:7]:[c:6]:[n;H0;D3;+0:5](-[CH;D3;+0:1]2-[C:2]-[C:3]-[C:4]-2):[c:10]:1
92
[{"value": 92.0, "product": "C1(CCC1)N1C=NC(=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.7, "product": "C1(CCC1)N1C=NC(=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
1,4-Dinitroimidazole (237 mg, 1.5 mmol, J. Phys. Chem. 1995, 99, 5009–5015) was added to a solution of cyclobutylamine (107 mg, 1.5 mmol) in methanol (10 mL) at 23° C. The reaction mixture was stirred for 16 h, then the solvent was removed in vacuo and the resulting residue was purified by silica gel chromatography (1:...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Primary amine
null
C1CCC1.c1c[nH]cn1
c1c[nH]cn1.C1CCC1
c1c[nH]cn1.C1CCC1
HO-
CO
null
16
NC1CCC1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1>CO>O=[N+]([O-])c1cn(C2CCC2)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-394e4d26bd894add8e909419ab362dae
NC1CCCC1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1>>O=[N+]([O-])c1cn(C2CCCC2)cn1
C1(CCCC1)N.[N+](=O)([O-])N1C=NC(=C1)[N+](=O)[O-]>>C1(CCCC1)N1C=NC(=C1)[N+](=O)[O-]
N[CH:7]1[CH2:8][CH2:9][CH2:10][CH2:11]1.O=[N+]([O-])[n:6]1[cH:5][c:4]([N+:2](=[O:1])[O-:3])[n:13][cH:12]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6]([CH:7]2[CH2:8][CH2:9][CH2:10][CH2:11]2)[cH:12][n:13]1
NC1CCCC1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1
O=[N+]([O-])c1cn(C2CCCC2)cn1
null
null
null
Functional Group Addition
OtherReaction
e919eded286ceea592f7af5daf8bf9d98ce3e82e260913bddabbbd1919ae9b8e
e44bfec7c64c2106b9732634e34828e6460a6db63dcf75ef4a78a1aabdfc680a
c1cn(C2CCCC2)cn1
N-[CH;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1.O=[N+](-[O-])-[n;H0;D3;+0:6]1:[c:7]:[#7;a:8]:[c:9](-[#7;+:10]):[c:11]:1>>[#7;+:10]-[c:9]1:[#7;a:8]:[c:7]:[n;H0;D3;+0:6](-[CH;D3;+0:1]2-[C:2]-[C:3]-[C:4]-[C:5]-2):[c:11]:1
75
[{"value": 75.0, "product": "C1(CCCC1)N1C=NC(=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
This reaction was carried out using the procedure for Preparation 1 with cyclopentyl amine and 1,4-dinitroimidazole to afford 205 mg (75% yield) of 1-cyclopentyl-4-nitro-1H-imidazole; 1H NMR (400 MHz, CDCl3) δ 7.77 (s, 1H), 7.45 (s, 1H), 4.49 (m, 1H), 2.25 (m, 2H), 2.0–1.7 (m, 6H); MS (AP/CI): 182.2 (M+H)+. Conditions:...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Primary amine
null
C1CCCC1.c1c[nH]cn1
c1c[nH]cn1.C1CCCC1
c1c[nH]cn1.C1CCCC1
HO-
null
null
null
NC1CCCC1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1>>O=[N+]([O-])c1cn(C2CCCC2)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1df8f83e785247e7b00c28cbc83a7c8b
N[C@H]1C[C@@H](c2ccccc2)C1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1>>O=[N+]([O-])c1cn([C@H]2C[C@@H](c3ccccc3)C2)cn1
C1(=CC=CC=C1)[C@H]1C[C@H](C1)N.[N+](=O)([O-])N1C=NC(=C1)[N+](=O)[O-]>>[N+](=O)([O-])C=1N=CN(C1)[C@@H]1C[C@@H](C1)C1=CC=CC=C1
N[C@H:7]1[CH2:8][C@@H:9]([c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)[CH2:16]1.O=[N+]([O-])[n:6]1[cH:5][c:4]([N+:2](=[O:1])[O-:3])[n:18][cH:17]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6]([C@H:7]2[CH2:8][C@@H:9]([c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[CH2:16]2)[cH:17][n:18]1
N[C@H]1C[C@@H](c2ccccc2)C1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1
O=[N+]([O-])c1cn([C@H]2C[C@@H](c3ccccc3)C2)cn1
null
null
null
Functional Group Addition
OtherReaction
46a51f8ca5a006fa0c7307aff9c47bbfab60ab29424e07318a72cc160ef81c35
e44bfec7c64c2106b9732634e34828e6460a6db63dcf75ef4a78a1aabdfc680a
c1ccc([C@H]2C[C@@H](n3ccnc3)C2)cc1
N-[C@@H;D3;+0:1]1-[C:2]-[C:3]-[C:4]-1.O=[N+](-[O-])-[n;H0;D3;+0:5]1:[c:6]:[#7;a:7]:[c:8](-[#7;+:9]):[c:10]:1>>[#7;+:9]-[c:8]1:[#7;a:7]:[c:6]:[n;H0;D3;+0:5](-[C@@H;D3;+0:1]2-[C:2]-[C:3]-[C:4]-2):[c:10]:1
46
[{"value": 46.0, "product": "[N+](=O)([O-])C=1N=CN(C1)[C@@H]1C[C@@H](C1)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
This reaction was carried out using the procedure for Preparation 1 with cis-3-phenylcyclobutylamine (J. Med. Pharm. Chem. 1960, 2, 687–691; ACIEE 1981, 20, 879–880) and 1,4-dinitroimidazole to afford 46 mg (46% yield) of 4-nitro-1-(cis-3-phenyl-cyclobutyl)-1H-imidazole; 1H NMR (300 MHz, CDCl3) δ 7.9 (s, 1H), 7.55 (s, ...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Primary amine
null
C1CCC1.c1c[nH]cn1
c1c[nH]cn1.C1CCC1
c1c[nH]cn1.C1CCC1.c1ccccc1
HO-
null
null
null
N[C@H]1C[C@@H](c2ccccc2)C1.O=[N+]([O-])c1cn([N+](=O)[O-])cn1>>O=[N+]([O-])c1cn([C@H]2C[C@@H](c3ccccc3)C2)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ab61f7c1bcb940689fe79b727d5479f0
O=C(O)Cc1ccc2ncccc2c1.O=[N+]([O-])c1cn(C2CCC2)cn1>>O=C(Cc1ccc2ncccc2c1)Nc1cn(C2CCC2)cn1
N1=CC=CC2=CC(=CC=C12)CC(=O)O.C1(CCC1)N1C=NC(=C1)[N+](=O)[O-].C(C)(=O)OCC.CCN(CC)CC>>C1(CCC1)N1C=NC(=C1)NC(CC=1C=C2C=CC=NC2=CC1)=O
O[C:2](=[O:1])[CH2:3][c:4]1[cH:5][cH:6][c:7]2[n:8][cH:9][cH:10][cH:11][c:12]2[cH:13]1.O=[N+:14]([O-])[c:15]1[cH:16][n:17]([CH:18]2[CH2:19][CH2:20][CH2:21]2)[cH:22][n:23]1>>[O:1]=[C:2]([CH2:3][c:4]1[cH:5][cH:6][c:7]2[n:8][cH:9][cH:10][cH:11][c:12]2[cH:13]1)[NH:14][c:15]1[cH:16][n:17]([CH:18]2[CH2:19][CH2:20][CH2:21]2)[c...
O=C(O)Cc1ccc2ncccc2c1.O=[N+]([O-])c1cn(C2CCC2)cn1
O=C(Cc1ccc2ncccc2c1)Nc1cn(C2CCC2)cn1
null
[Pd]
C(Cl)Cl
Acylation
OtherReaction
07d1695adb57fcbe166e427114577c880df19df2ee26bdadcbdf979c1785ff55
141f63f004bbbe912fc54e457ad7143d740953538a28293f72b74ca32c03fab9
O=C(Cc1ccc2ncccc2c1)Nc1cn(C2CCC2)cn1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4].O=[N+;H0;D3:5](-[O-])-[c:6]1:[#7;a:7]:[c:8]:[#7;a:9](-[C:10]):[c:11]:1>>[C:10]-[#7;a:9]1:[c:11]:[c:6](-[NH;D2;+0:5]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4]):[#7;a:7]:[c:8]:1
47.1
[{"value": 47.0, "product": "C1(CCC1)N1C=NC(=C1)NC(CC=1C=C2C=CC=NC2=CC1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 47.1, "product": "C1(CCC1)N1C=NC(=C1)NC(CC=1C=C2C=CC=NC2=CC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-10
CELSIUS
2
HOUR
To a Parr hydrogenation bottle was added 1-cyclobutyl-4-nitro-1H-imidazole (Preparation 1, 150 mg, 0.9 mmol) and ethyl acetate (10 mL), followed by 10% Pd on carbon (250 mg). The reaction mixture was placed on a Parr hydrogenation apparatus and was reacted for 6 h under 50 psi H2 at 23° C. The contents of the bottle we...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Nitro group
Secondary amide
null
null
c1ccc2ncccc2c1.c1c[nH]cn1.C1CCC1
Other
[Pd].C(Cl)Cl
-10
2
O=C(O)Cc1ccc2ncccc2c1.O=[N+]([O-])c1cn(C2CCC2)cn1>[Pd].C(Cl)Cl>O=C(Cc1ccc2ncccc2c1)Nc1cn(C2CCC2)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bf88feb4393b4c36bcb3236484326876
O=C(Cl)Oc1ccccc1.O=[N+]([O-])c1cn(C2CCC2)cn1>>O=C(Nc1cn(C2CCC2)cn1)Oc1ccccc1
C1(=CC=CC=C1)OC(=O)Cl.C(C)(=O)O.C(C)(C)N(CC)C(C)C.C1(CCC1)N1C=NC(=C1)[N+](=O)[O-]>>C1(=CC=CC=C1)OC(NC=1N=CN(C1)C1CCC1)=O
Cl[C:2](=[O:1])[O:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1.O=[N+:3]([O-])[c:4]1[cH:5][n:6]([CH:7]2[CH2:8][CH2:9][CH2:10]2)[cH:11][n:12]1>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][n:6]([CH:7]2[CH2:8][CH2:9][CH2:10]2)[cH:11][n:12]1)[O:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1
O=C(Cl)Oc1ccccc1.O=[N+]([O-])c1cn(C2CCC2)cn1
O=C(Nc1cn(C2CCC2)cn1)Oc1ccccc1
null
[Pd]
CO.C(C)(=O)OCC
Functional Group Interconversion
OtherReaction
621586d13f370c21d9c2ebcb2ff6f006e9ee7ea1c7077f0238750d1cd3d6b3c1
1634e3af8fcf6a1e120353a67242b0b2217479df5f77fe48e17bc4747cae1639
O=C(Nc1cn(C2CCC2)cn1)Oc1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[c:4].O=[N+;H0;D3:5](-[O-])-[c:6]1:[#7;a:7]:[c:8]:[#7;a:9](-[C:10]):[c:11]:1>>[C:10]-[#7;a:9]1:[c:8]:[#7;a:7]:[c:6](-[NH;D2;+0:5]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[c:4]):[c:11]:1
72
[{"value": 65.0, "product": "C1(=CC=CC=C1)OC(NC=1N=CN(C1)C1CCC1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.0, "product": "C1(=CC=CC=C1)OC(NC=1N=CN(C1)C1CCC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
6
HOUR
A Parr hydrogenation bottle was charged with 1-cyclobutyl-4-nitro-1H-imidazole (Preparation 1, 3 g, 18 mmol) and ethyl acetate (70 mL) followed by 10% Pd on carbon (1.2 g) under a nitrogen atmosphere. The mixture was hydrogenated for 6 h under 50 psi H2 at 23° C. The mixture was then filtered through a pad of celite wh...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether.Nitro group
Carbamic ester
null
null
c1c[nH]cn1.C1CCC1.c1ccccc1
Other
[Pd].CO.C(C)(=O)OCC
-78
6
O=C(Cl)Oc1ccccc1.O=[N+]([O-])c1cn(C2CCC2)cn1>[Pd].CO.C(C)(=O)OCC>O=C(Nc1cn(C2CCC2)cn1)Oc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-93263c435c93462daf7f5cb4f36258a7
Nc1cccc2cnccc12.O=C(Nc1cn(C2CCC2)cn1)Oc1ccccc1>>O=C(Nc1cn(C2CCC2)cn1)Nc1cccc2cnccc12
C1(=CC=CC=C1)OC(NC=1N=CN(C1)C1CCC1)=O.NC1=C2C=CN=CC2=CC=C1>>C1(CCC1)N1C=NC(=C1)NC(=O)NC1=C2C=CN=CC2=CC=C1
[NH2:13][c:14]1[cH:15][cH:16][cH:17][c:18]2[cH:19][n:20][cH:21][cH:22][c:23]12.c1ccc(O[C:2](=[O:1])[NH:3][c:4]2[cH:5][n:6]([CH:7]3[CH2:8][CH2:9][CH2:10]3)[cH:11][n:12]2)cc1>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][n:6]([CH:7]2[CH2:8][CH2:9][CH2:10]2)[cH:11][n:12]1)[NH:13][c:14]1[cH:15][cH:16][cH:17][c:18]2[cH:19][n:20][cH:21][c...
Nc1cccc2cnccc12.O=C(Nc1cn(C2CCC2)cn1)Oc1ccccc1
O=C(Nc1cn(C2CCC2)cn1)Nc1cccc2cnccc12
null
null
O1CCOCC1.CN(C)C=O
Acylation
OtherReaction
f934f97c87bbca35fb6a2e4d8038127ebfc978d6e7ce352fd6acc2bdfa51d605
d200d0a31426bb545e5b3d618baa98893432cc10661e9fc97221c430e6ae866e
O=C(Nc1cn(C2CCC2)cn1)Nc1cccc2cnccc12
[#7;a:1]:[c:2](-[#7:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-O-c1:c:c:c:c:c:1):[c:6]:[#7;a:7].[NH2;D1;+0:8]-[c:9](:[c:10]):[c:11]>>[#7;a:1]:[c:2](-[#7:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[NH;D2;+0:8]-[c:9](:[c:10]):[c:11]):[c:6]:[#7;a:7]
52
[{"value": 52.0, "product": "C1(CCC1)N1C=NC(=C1)NC(=O)NC1=C2C=CN=CC2=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 51.4, "product": "C1(CCC1)N1C=NC(=C1)NC(=O)NC1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
null
null
To a 1 dram vial with septa screw cap was added (1-cyclobutyl-1H-imidazol-4-yl)-carbamic acid phenyl ester (Example 4, 50 mg, 0.19 mmol), 5-aminoisoquinoline (30 mg, 0.21 mmol), and 1:1 dioxane-DMF (1 mL). The reaction mixture was heated at 70° C. for 2 h. The reaction mixture was adsorbed onto silica gel and was purif...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Primary amine
Urea
c1ccccc1
null
c1c[nH]cn1.C1CCC1.c1ccc2cnccc2c1
HO-
O1CCOCC1.CN(C)C=O
70
null
Nc1cccc2cnccc12.O=C(Nc1cn(C2CCC2)cn1)Oc1ccccc1>O1CCOCC1.CN(C)C=O>O=C(Nc1cn(C2CCC2)cn1)Nc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-496b10fd4f3f4c06b178e187ca96e743
Cc1ccc(S(=O)(=O)Cl)cc1.O=[N+]([O-])c1cn(C2CC(O)C2)cn1>>Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc([N+](=O)[O-])c3)C2)cc1
[N+](=O)([O-])C=1N=CN(C1)C1CC(C1)O.CCN(CC)CC.C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>[N+](=O)([O-])C=1N=CN(C1)[C@@H]1C[C@H](C1)OS(=O)(=O)C1=CC=C(C=C1)C
Cl[S:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:23][cH:22]1)(=[O:7])=[O:8].[OH:9][CH:10]1[CH2:11][CH:12]([n:13]2[cH:14][n:15][c:16]([N+:17](=[O:18])[O-:19])[cH:20]2)[CH2:21]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[O:9][C@H:10]2[CH2:11][C@H:12]([n:13]3[cH:14][n:15][c:16]([N+:17](=[O:18])[O-:19])[cH:20]3)[CH2:...
Cc1ccc(S(=O)(=O)Cl)cc1.O=[N+]([O-])c1cn(C2CC(O)C2)cn1
Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc([N+](=O)[O-])c3)C2)cc1
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
ad3deb6f5d4dc7823aa3ad2bfe24985be1f3e6860ff8cc0ba215d7624074ef69
ec645297cfd3107bffb1a4753ac125e48856598e58005e939bb2f0e91bf5e57c
O=S(=O)(O[C@H]1C[C@H](n2ccnc2)C1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[OH;D1;+0:7]-[CH;D3;+0:8]1-[C:9]-[C:10]-[C:11]-1>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[O;H0;D2;+0:7]-[C@@H;D3;+0:8]1-[C:9]-[C:10]-[C:11]-1)-[c:4](:[c:5]):[c:6]
37
[{"value": 37.0, "product": "[N+](=O)([O-])C=1N=CN(C1)[C@@H]1C[C@H](C1)OS(=O)(=O)C1=CC=C(C=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 36.4, "product": "[N+](=O)([O-])C=1N=CN(C1)[C@@H]1C[C@H](C1)OS(=O)(=O)C1=CC=C(C=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
3-(4-nitro-imidazol-1-yl)-cyclobutanol (Preparation 4, Step 1; 4 g, 22 mmol) was treated with Et3N (7.7 mL, 55 mmol) in methylene chloride (150 mL) followed by p-toluenesulfonyl chloride (TsCl) (5 g, 26.4 mmol) and 4-N,N-dimethylaminopyridine (DMAP) (268 mg, 2.2 mmol). The resulting mixture was stirred at room temperat...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Secondary alcohol.Sulfonyl halide
Tosylate
null
null
c1ccccc1.C1CCC1.c1c[nH]cn1
HCl
C(Cl)Cl
null
24
Cc1ccc(S(=O)(=O)Cl)cc1.O=[N+]([O-])c1cn(C2CC(O)C2)cn1>C(Cl)Cl>Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc([N+](=O)[O-])c3)C2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-513e4b24fd25466eb922d5cf54934be7
Cc1ccc(S(=O)(=O)O[C@@H]2C[C@H](n3cnc([N+](=O)[O-])c3)C2)cc1.O=C(O)Cc1cccc2ccccc12>>Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)cc1
[N+](=O)([O-])C=1N=CN(C1)[C@H]1C[C@H](C1)OS(=O)(=O)C1=CC=C(C=C1)C.CCN(CC)CC.C1(=CC=CC2=CC=CC=C12)CC(=O)O>>C1(=CC=CC2=CC=CC=C12)CC(=O)NC=1N=CN(C1)[C@@H]1C[C@H](C1)OS(=O)(=O)C1=CC=C(C=C1)C
O=[N+:17]([O-])[c:16]1[n:15][cH:14][n:13]([C@@H:12]2[CH2:11][C@H:10]([O:9][S:6]([c:5]3[cH:4][cH:3][c:2]([CH3:1])[cH:34][cH:33]3)(=[O:7])=[O:8])[CH2:32]2)[cH:31]1.O[C:18](=[O:19])[CH2:20][c:21]1[cH:22][cH:23][cH:24][c:25]2[cH:26][cH:27][cH:28][cH:29][c:30]12>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[O:9][C@H...
Cc1ccc(S(=O)(=O)O[C@@H]2C[C@H](n3cnc([N+](=O)[O-])c3)C2)cc1.O=C(O)Cc1cccc2ccccc12
Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)cc1
null
[Pd]
C(C)(=O)OCC
Acylation
OtherReaction
07d1695adb57fcbe166e427114577c880df19df2ee26bdadcbdf979c1785ff55
141f63f004bbbe912fc54e457ad7143d740953538a28293f72b74ca32c03fab9
O=C(Cc1cccc2ccccc12)Nc1cn([C@H]2C[C@H](OS(=O)(=O)c3ccccc3)C2)cn1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4].O=[N+;H0;D3:5](-[O-])-[c:6]1:[#7;a:7]:[c:8]:[#7;a:9](-[C:10]):[c:11]:1>>[C:10]-[#7;a:9]1:[c:8]:[#7;a:7]:[c:6](-[NH;D2;+0:5]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4]):[c:11]:1
72.1
[{"value": 72.0, "product": "C1(=CC=CC2=CC=CC=C12)CC(=O)NC=1N=CN(C1)[C@@H]1C[C@H](C1)OS(=O)(=O)C1=CC=C(C=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.1, "product": "C1(=CC=CC2=CC=CC=C12)CC(=O)NC=1N=CN(C1)[C@@H]1C[C@H](C1)OS(=O)(=O)C1=CC=C(C=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired...
null
null
1
HOUR
trans-Toluene-4-sulfonic acid 3-(4-nitro-imidazol-1-yl)-cyclobutyl ester (Preparation 4, Step 2; 590 mg, 1.75 mmol) was mixed with 10% Pd on carbon (500 mg) in ethyl acetate (30 mL). The mixture was then reacted under 50 psi H2 at room temperature for 6 h. The mixture was filtered through celite into a flame-dried flas...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Nitro group
Secondary amide
null
null
c1ccccc1.C1CCC1.c1c[nH]cn1.c1ccc2ccccc2c1
Other
[Pd].C(C)(=O)OCC
null
1
Cc1ccc(S(=O)(=O)O[C@@H]2C[C@H](n3cnc([N+](=O)[O-])c3)C2)cc1.O=C(O)Cc1cccc2ccccc12>[Pd].C(C)(=O)OCC>Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6b141b9602e2484784b713018045e405
Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)cc1.[N-]=[N+]=[N-]>>[N-]=[N+]=N[C@@H]1C[C@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1
C1(=CC=CC2=CC=CC=C12)CC(=O)NC=1N=CN(C1)[C@@H]1C[C@H](C1)OS(=O)(=O)C1=CC=C(C=C1)C.[N-]=[N+]=[N-].[Na+].C(Cl)(Cl)Cl>>N(=[N+]=[N-])[C@H]1C[C@H](C1)N1C=NC(=C1)NC(CC1=CC=CC2=CC=CC=C12)=O
Cc1ccc(S(=O)(=O)O[C@H:4]2[CH2:5][C@H:6]([n:7]3[cH:8][n:9][c:10]([NH:11][C:12](=[O:13])[CH2:14][c:15]4[cH:16][cH:17][cH:18][c:19]5[cH:20][cH:21][cH:22][cH:23][c:24]45)[cH:25]3)[CH2:26]2)cc1.[N-:1]=[N+:2]=[N-:3]>>[N-:1]=[N+:2]=[N:3][C@H:4]1[CH2:5][C@@H:6]([n:7]2[cH:8][n:9][c:10]([NH:11][C:12](=[O:13])[CH2:14][c:15]3[cH:1...
Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)cc1.[N-]=[N+]=[N-]
[N-]=[N+]=N[C@@H]1C[C@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1
null
null
O.C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
fe84f7dc4a5324b680ee11df06675b930381f67a207b8a43b5bbf96a6445c757
6961229e10e0db3c410e97098a5b94923cb09bb1c069f267ae4410afd98cc24e
O=C(Cc1cccc2ccccc12)Nc1cn(C2CCC2)cn1
C-c1:c:c:c(-S(=O)(=O)-O-[C@@H;D3;+0:1]2-[C:2]-[C:3]-[C:4]-2):c:c:1.[N-;H0;D1:5]=[#7;+:6]=[N;-;D1;H0:7]>>[N;-;D1;H0:7]=[#7;+:6]=[N;H0;D2;+0:5]-[C@@H;D3;+0:1]1-[C:2]-[C:3]-[C:4]-1
79
[{"value": 79.0, "product": "N(=[N+]=[N-])[C@H]1C[C@H](C1)N1C=NC(=C1)NC(CC1=CC=CC2=CC=CC=C12)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.5, "product": "N(=[N+]=[N-])[C@H]1C[C@H](C1)N1C=NC(=C1)NC(CC1=CC=CC2=CC=CC=C12)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
96
HOUR
trans-Toluene-4-sulfonic acid 3-[4-(2-naphthalen-1-yl-acetylamino)-imidazol-1-yl]-cyclobutyl ester (Preparation 4, Step 3; 593 mg, 1.25 mmol) was mixed with sodium azide (813 mg, 12.5 mmol) in ethanol (15 mL), water (5 mL), and chloroform (5 mL). The mixture was then heated at reflux with stirring for 96 h. The solvent...
10.6084/m9.figshare.5104873.v1
null
Tosylate
Azide
c1ccccc1.C1CCC1
C1CCC1
C1CCC1.c1c[nH]cn1.c1ccc2ccccc2c1
TsOH.HO-
O.C(C)O
null
96
Cc1ccc(S(=O)(=O)O[C@@H]2C[C@@H](n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)cc1.[N-]=[N+]=[N-]>O.C(C)O>[N-]=[N+]=N[C@@H]1C[C@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2336ab26e4584b5fb49276c5b188bb19
[N-]=[N+]=N[C@@H]1C[C@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1>>N[C@H]1C[C@@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1
N(=[N+]=[N-])[C@H]1C[C@H](C1)N1C=NC(=C1)NC(CC1=CC=CC2=CC=CC=C12)=O.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>N[C@H]1C[C@H](C1)N1C=NC(=C1)NC(CC1=CC=CC2=CC=CC=C12)=O
[N-]=[N+]=[N:1][C@H:2]1[CH2:3][C@@H:4]([n:5]2[cH:6][n:7][c:8]([NH:9][C:10](=[O:11])[CH2:12][c:13]3[cH:14][cH:15][cH:16][c:17]4[cH:18][cH:19][cH:20][cH:21][c:22]34)[cH:23]2)[CH2:24]1>>[NH2:1][C@H:2]1[CH2:3][C@@H:4]([n:5]2[cH:6][n:7][c:8]([NH:9][C:10](=[O:11])[CH2:12][c:13]3[cH:14][cH:15][cH:16][c:17]4[cH:18][cH:19][cH:2...
[N-]=[N+]=N[C@@H]1C[C@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1
N[C@H]1C[C@@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1
null
null
O1CCCC1.O
Reduction
Azide to amine reduction (Staudinger)
4c9e4990dae2bb965dec06bd45e318560989ee3681b61e443f7aa363b7cfa222
cd009d687d606bf351eac9390a176d16be38f2c8216a599b398641009c215027
O=C(Cc1cccc2ccccc12)Nc1cn(C2CCC2)cn1
[C:1]-[C:2](-[N;H0;D2;+0:3]=[N+]=[N-])-[C:4]>>[C:1]-[C:2](-[NH2;D1;+0:3])-[C:4]
95
[{"value": 95.0, "product": "N[C@H]1C[C@H](C1)N1C=NC(=C1)NC(CC1=CC=CC2=CC=CC=C12)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.0, "product": "N[C@H]1C[C@H](C1)N1C=NC(=C1)NC(CC1=CC=CC2=CC=CC=C12)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
N-[1-(cis-3-azido-cyclobutyl)-1H-imidazol-4-yl]-2-naphthalen-1-yl-acetamide (Preparation 4, Step 4; 330 mg, 0.95 mmol) was treated with triphenylphosphine (301 mg, 1.15 mmol) in tetrahydrofuran (10 mL) and water (1 mL) at 23° C. The solution was stirred at room temperature for 18 h. The solvent was removed in vacuo and...
10.6084/m9.figshare.5104873.v1
null
Azide
Primary amine
null
null
C1CCC1.c1c[nH]cn1.c1ccc2ccccc2c1
Other
O1CCCC1.O
null
18
[N-]=[N+]=N[C@@H]1C[C@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1>O1CCCC1.O>N[C@H]1C[C@@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-12cb8a95f5ef4ea8885b99cd70a92718
Cc1cccc(C(=O)O)n1.N[C@H]1C[C@@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1>>Cc1cccc(C(=O)NC2CC(n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)n1
[OH-].[Na+].CC1=CC=CC(=N1)C(=O)O.Cl.CN(CCCN=C=NCC)C.N[C@H]1C[C@H](C1)N1C=NC(=C1)NC(CC1=CC=CC2=CC=CC=C12)=O>>C1(=CC=CC2=CC=CC=C12)CC(=O)NC=1N=CN(C1)C1CC(C1)NC(=O)C1=NC(=CC=C1)C
O[C:7]([c:6]1[cH:5][cH:4][cH:3][c:2]([CH3:1])[n:33]1)=[O:8].[NH2:9][C@H:10]1[CH2:11][C@@H:12]([n:13]2[cH:14][n:15][c:16]([NH:17][C:18](=[O:19])[CH2:20][c:21]3[cH:22][cH:23][cH:24][c:25]4[cH:26][cH:27][cH:28][cH:29][c:30]34)[cH:31]2)[CH2:32]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]([C:7](=[O:8])[NH:9][CH:10]2[CH2:11][CH:1...
Cc1cccc(C(=O)O)n1.N[C@H]1C[C@@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1
Cc1cccc(C(=O)NC2CC(n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)n1
null
CN(C)C=1C=CN=CC1
O.C(Cl)Cl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(Cc1cccc2ccccc12)Nc1cn(C2CC(NC(=O)c3ccccn3)C2)cn1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#7;a:5]:[c:6].[NH2;D1;+0:7]-[C@@H;D3;+0:8]1-[C:9]-[C:10]-[C:11]-1>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[NH;D2;+0:7]-[CH;D3;+0:8]1-[C:9]-[C:10]-[C:11]-1)-[c:3](:[c:4]):[#7;a:5]:[c:6]
98.6
[{"value": 95.0, "product": "C1(=CC=CC2=CC=CC=C12)CC(=O)NC=1N=CN(C1)C1CC(C1)NC(=O)C1=NC(=CC=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.6, "product": "C1(=CC=CC2=CC=CC=C12)CC(=O)NC=1N=CN(C1)C1CC(C1)NC(=O)C1=NC(=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
A solution of 6-methylpicolinic acid (9.4 mg, 0.07 mmol) in methylene chloride was treated with 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (84 mg) and DMAP (2 mg) at 23° C. After stirring for 10 min, N-[1-(cis-3-amino-cyclobutyl)-1H-imidazol-4-yl]-2-naphthalen-1-yl-acetamide (Example 6, 20 mg, 0.06 mmo...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccncc1.C1CCC1.c1c[nH]cn1.c1ccc2ccccc2c1
HO-
CN(C)C=1C=CN=CC1.O.C(Cl)Cl
null
0.166667
Cc1cccc(C(=O)O)n1.N[C@H]1C[C@@H](n2cnc(NC(=O)Cc3cccc4ccccc34)c2)C1>CN(C)C=1C=CN=CC1.O.C(Cl)Cl>Cc1cccc(C(=O)NC2CC(n3cnc(NC(=O)Cc4cccc5ccccc45)c3)C2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9f844d6be33f44678c9fb02776f3567e
Br.Nc1cccc2cnccc12>>Brc1cccc2cnccc12
[OH-].[K+].N(=O)[O-].[Na+].NC1=C2C=CN=CC2=CC=C1.Br>>BrC1=C2C=CN=CC2=CC=C1
[BrH:1].N[c:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][n:8][cH:9][cH:10][c:11]12>>[Br:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][n:8][cH:9][cH:10][c:11]12
Br.Nc1cccc2cnccc12
Brc1cccc2cnccc12
null
[Cu]
O
Miscellaneous
OtherReaction
a80b46bfc720178a7247f763a2a5c279a0921fee09e9f9f15b3416ca42dac62e
1129c10513c603d2647e51dd9713063aaf10bd8a364ed275b9b93c32624e3ba4
c1ccc2cnccc2c1
N-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[BrH;D0;+0:10]>>[Br;H0;D1;+0:10]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
53
[{"value": 53.0, "product": "BrC1=C2C=CN=CC2=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
-78
CELSIUS
15
MINUTE
5-Aminoisoquinoline (5.0 g, 34.7 mmol) was mixed with 48% aqueous HBr (65 mL) at −78° C. for 15 min. Sodium nitrite (3.1 g, 45 mmol) in water (6 mL) was then added dropwise. After stirring for 15 min at −78° C., the mixture was warmed to 0° C. Copper powder (0.3 g) was added very slowly to avoid excessive foaming. Afte...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Aromatic halide
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
Other
[Cu].O
-78
0.25
Br.Nc1cccc2cnccc12>[Cu].O>Brc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-45852c4d4052420286b592d39aa1fdb0
Brc1cccc2cnccc12.C=C[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC>>C=CCc1cccc2cnccc12
BrC1=C2C=CN=CC2=CC=C1.C(C=C)[Sn](CCCC)(CCCC)CCCC.[F-].[K+]>>C(C=C)C1=C2C=CN=CC2=CC=C1
Br[c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12.CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2:3][CH:2]=[CH2:1]>>[CH2:1]=[CH:2][CH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12
Brc1cccc2cnccc12.C=C[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC
C=CCc1cccc2cnccc12
null
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.Cl[Pd]Cl
C1(=CC=CC=C1)C
C-C Coupling
Stille reaction_allyl
3d6f296cd1217b6cb0262306f30301e2261b84eea5090d90b511755d78d7700c
1bc148b1555a9c8fc11becbecded2f430d1be44535a8bef8d1f9251cc75697a6
c1ccc2cnccc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.C-C-C-[CH2]-[Sn](-[CH2;D2;+0:10]-[C:11]=[C;D1;H2:12])(-[CH2]-C-C-C)-[CH2]-C-C-C>>[C;D1;H2:12]=[C:11]-[CH2;D2;+0:10]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
92
[{"value": 92.0, "product": "C(C=C)C1=C2C=CN=CC2=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.9, "product": "C(C=C)C1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
5-Bromoisoquinoline (Preparation 6, Step 1, 1.04 g, 5.0 mmol) was mixed with allyltributyltin (1.7 mL, 5.5 mmol) and dichloropalladium bis(triphenylphosphine) (176 mg, 0.25 mmol) in toluene (20 mL) under a nitrogen atmosphere. The mixture was heated at reflux for 16 h. After cooling to room temperature, a saturated aqu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Allyl.Tin
Allyl
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HBr.Sn
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.Cl[Pd]Cl.C1(=CC=CC=C1)C
null
0.25
Brc1cccc2cnccc12.C=C[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC>C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.Cl[Pd]Cl.C1(=CC=CC=C1)C>C=CCc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5e769c17b7c64d7f898e6a8d4ec550c4
C=CCc1cccc2cnccc12.CO.[O]=[Mn](=[O])(=[O])[O-]>>COC(=O)Cc1cccc2cnccc12
[O-][Mn](=O)(=O)=O.[K+].C(C=C)C1=C2C=CN=CC2=CC=C1.O.CO.C(CO)O>>COC(CC1=C2C=CN=CC2=CC=C1)=O
C=[CH:3][CH2:5][c:6]1[cH:7][cH:8][cH:9][c:10]2[cH:11][n:12][cH:13][cH:14][c:15]12.[CH3:1][OH:2].[O]=[Mn](=[O])([O-])=[O:4]>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][c:6]1[cH:7][cH:8][cH:9][c:10]2[cH:11][n:12][cH:13][cH:14][c:15]12
C=CCc1cccc2cnccc12.CO.[O]=[Mn](=[O])(=[O])[O-]
COC(=O)Cc1cccc2cnccc12
null
null
C(C)(=O)O.C(Cl)Cl
Acylation
OtherReaction
51213de6b1433e32dc9d7d7afe9913992311eb89aa044c5216885e6b098219cb
446cb7d8dc7cecea3abe2b1ac52def3cf663d88a77e1b0a85a7a3d919f272021
c1ccc2cnccc2c1
C=[CH;D2;+0:1]-[C:2]-[c:3].[C;D1;H3:4]-[OH;D1;+0:5].[O-]-[Mn](=[O;H0;D1;+0:6])(=[O])=[O]>>[C;D1;H3:4]-[O;H0;D2;+0:5]-[C;H0;D3;+0:1](=[O;H0;D1;+0:6])-[C:2]-[c:3]
null
[]
0
CELSIUS
18
HOUR
5-Allylisoquinoline (Preparation 6, Step 2; 169 mg, 1.0 mmol) in methylene chloride (2 mL), acetic acid (0.5 mL), and water (0.5 mL) was treated with dimethyl polyethylene glycol (Mn ca. 500, 95 uL, 100 mg, 0.2 mmol) in methylene chloride (1 mL) at 23° C. The mixture was cooled to 0° C. and powdered KMnO4 (521 mg, 3.3 ...
10.6084/m9.figshare.5104873.v1
null
Allyl.Methanol
Ester
null
null
c1ccc2cnccc2c1
HO-
C(C)(=O)O.C(Cl)Cl
0
18
C=CCc1cccc2cnccc12.CO.[O]=[Mn](=[O])(=[O])[O-]>C(C)(=O)O.C(Cl)Cl>COC(=O)Cc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cb8eabb9955f4cb8ac74a6e293ab6ba3
COC(=O)Cc1cccc2cnccc12>>O=C(O)Cc1cccc2cnccc12
COC(CC1=C2C=CN=CC2=CC=C1)=O.[OH-].[Na+]>>C1=NC=CC2=C(C=CC=C12)CC(=O)O
C[O:3][C:2](=[O:1])[CH2:4][c:5]1[cH:6][cH:7][cH:8][c:9]2[cH:10][n:11][cH:12][cH:13][c:14]12>>[O:1]=[C:2]([OH:3])[CH2:4][c:5]1[cH:6][cH:7][cH:8][c:9]2[cH:10][n:11][cH:12][cH:13][c:14]12
COC(=O)Cc1cccc2cnccc12
O=C(O)Cc1cccc2cnccc12
null
null
C(C)(=O)O
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc2cnccc2c1
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
47
[{"value": 47.0, "product": "C1=NC=CC2=C(C=CC=C12)CC(=O)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 41.7, "product": "C1=NC=CC2=C(C=CC=C12)CC(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
8
HOUR
Isoquinolin-5-yl-acetic acid methyl ester (Preparation 6, Step 3; 90 mg, 0.448 mmol) was treated with aqueous sodium hydroxide (4N, 3 mL) and the solution was heated at 50° C. for 4 h. The solution was cooled to 0° C. and acetic acid (2 mL) was added dropwise, which resulted in the formation of a precipitate. The mixtu...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccc2cnccc2c1
Other
C(C)(=O)O
50
8
COC(=O)Cc1cccc2cnccc12>C(C)(=O)O>O=C(O)Cc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a9dd66b024284e8ba5081694ebe1d0d1
CCOC(=O)C1=CCCCC1S(=O)(=O)Nc1ccc(F)cc1F.SCc1ccccc1>>CCOC(=O)C1=CCCCC1SCc1ccccc1
FC1=C(C=CC(=C1)F)NS(=O)(=O)C1CCCC=C1C(=O)OCC.C1(=CC=CC=C1)CS.C1CCC2=NCCCN2CC1>>C(C1=CC=CC=C1)SC1CCCC=C1C(=O)OCC
O=S(=O)(Nc1ccc(F)cc1F)[CH:11]1[C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])=[CH:7][CH2:8][CH2:9][CH2:10]1.[SH:12][CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]1=[CH:7][CH2:8][CH2:9][CH2:10][CH:11]1[S:12][CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1
CCOC(=O)C1=CCCCC1S(=O)(=O)Nc1ccc(F)cc1F.SCc1ccccc1
CCOC(=O)C1=CCCCC1SCc1ccccc1
null
null
CN(C=O)C.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
e004b55701497d7f887b0985a65eca3bb4adb702fb3d6e33c5b8a4e402b31ab3
cfa39748e584de8627741a4eb08a3e46f3d1f6ce86fafef224e3e259ec2309d6
C1=CC(SCc2ccccc2)CCC1
F-c1:c:c:c(-N-S(=O)(=O)-[CH;D3;+0:1]2-[C:2]-[C:3]-[C:4]-[C:5]=[C:6]-2-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]):c(-F):c:1.[SH;D1;+0:11]-[C:12]-[c:13]>>[C:10]-[#8:9]-[C:7](=[O;D1;H0:8])-[C:6]1=[C:5]-[C:4]-[C:3]-[C:2]-[CH;D3;+0:1]-1-[S;H0;D2;+0:11]-[C:12]-[c:13]
null
[]
null
null
18
HOUR
To a solution of ethyl 6-[N-(2,4-difluorophenyl)sulfamoyl]-1-cyclohexene-1-carboxylate (1 g, synthesized according to the method disclosed in JP-A-10-056492) and phenylmethanethiol (719 mg) in N,N-dimethylformamide (20 ml) was added dropwise under ice-cooling 1,8-diazabicyclo[5,4,0]-7-undecene (441 mg) and the mixture ...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Aromatic halide.Aromatic halide.Aliphatic thiol
Monosulfide
c1ccccc1.C1=CCCCC1
C1=CCCCC1
C1=CCCCC1.c1ccccc1
HF
CN(C=O)C.C(C)(=O)OCC
null
18
CCOC(=O)C1=CCCCC1S(=O)(=O)Nc1ccc(F)cc1F.SCc1ccccc1>CN(C=O)C.C(C)(=O)OCC>CCOC(=O)C1=CCCCC1SCc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1bdc4cc6fcb44052a3d901234294f8e6
CCOC(=O)C1=CCCCC1S(=O)(=O)Nc1ccc(F)cc1F.COc1ccc(CS)cc1>>CCOC(=O)C1=CCCCC1SCc1ccc(OC)cc1
FC1=C(C=CC(=C1)F)NS(=O)(=O)C1CCCC=C1C(=O)OCC.COC1=CC=C(C=C1)CS>>COC1=CC=C(CSC2CCCC=C2C(=O)OCC)C=C1
O=S(=O)(Nc1ccc(F)cc1F)[CH:11]1[C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])=[CH:7][CH2:8][CH2:9][CH2:10]1.[SH:12][CH2:13][c:14]1[cH:15][cH:16][c:17]([O:18][CH3:19])[cH:20][cH:21]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]1=[CH:7][CH2:8][CH2:9][CH2:10][CH:11]1[S:12][CH2:13][c:14]1[cH:15][cH:16][c:17]([O:18][CH3:19])[cH:20][cH:21...
CCOC(=O)C1=CCCCC1S(=O)(=O)Nc1ccc(F)cc1F.COc1ccc(CS)cc1
CCOC(=O)C1=CCCCC1SCc1ccc(OC)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
e004b55701497d7f887b0985a65eca3bb4adb702fb3d6e33c5b8a4e402b31ab3
cfa39748e584de8627741a4eb08a3e46f3d1f6ce86fafef224e3e259ec2309d6
C1=CC(SCc2ccccc2)CCC1
F-c1:c:c:c(-N-S(=O)(=O)-[CH;D3;+0:1]2-[C:2]-[C:3]-[C:4]-[C:5]=[C:6]-2-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]):c(-F):c:1.[SH;D1;+0:11]-[C:12]-[c:13]>>[C:10]-[#8:9]-[C:7](=[O;D1;H0:8])-[C:6]1=[C:5]-[C:4]-[C:3]-[C:2]-[CH;D3;+0:1]-1-[S;H0;D2;+0:11]-[C:12]-[c:13]
95.6
[{"value": 95.6, "product": "COC1=CC=C(CSC2CCCC=C2C(=O)OCC)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
In the same manner as in Reference Example 1, ethyl 6-[N-(2,4-difluorophenyl)sulfamoyl]-1-cyclohexene-1-carboxylate (1 g) and (4-methoxyphenyl)methanethiol (893 mg) were reacted to give ethyl 6-[(4-methoxybenzyl)-sulfanyl]-1-cyclohexene-1-carboxylate (848 mg) as a colorless oil. Conditions: See reaction.notes.procedure...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Aromatic halide.Aromatic halide.Aliphatic thiol
Monosulfide
c1ccccc1.C1=CCCCC1
C1=CCCCC1
C1=CCCCC1.c1ccccc1
HF
null
null
null
CCOC(=O)C1=CCCCC1S(=O)(=O)Nc1ccc(F)cc1F.COc1ccc(CS)cc1>>CCOC(=O)C1=CCCCC1SCc1ccc(OC)cc1