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36
36
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4
873
rxn_insight_reaction
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19
1.07k
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14
3.37k
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1
581
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1
433
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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
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large_stringlengths
64
64
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large_stringlengths
5
288
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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
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3 values
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float64
0
4k
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4 values
procedure_details
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1
23.6k
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96 values
doi
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large_stringlengths
3
716
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large_stringlengths
3
539
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large_stringlengths
5
293
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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
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float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1218cddf6284426e962b405ad48bf739
COC(=O)c1cc(-c2ccc(OC)c(F)c2)n[nH]c1=O.ClCC=Cc1ccc(Cl)cc1>>COC(=O)c1cc(-c2ccc(OC)c(F)c2)nn(CC=Cc2ccc(Cl)cc2)c1=O
FC1=C(C=CC(=C1)F)C=1C=C(C(N(N1)CC(C)C)=O)CO.FC=1C=C(C=CC1OC)C=1C=C(C(NN1)=O)C(=O)OC.ClC1=CC=C(C=CCCl)C=C1>>ClC1=CC=C(C=CCN2N=C(C=C(C2=O)C(=O)OC)C2=CC(=C(C=C2)OC)F)C=C1
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([O:12][CH3:13])[c:14]([F:15])[cH:16]2)[n:17][nH:18][c:29]1=[O:30].Cl[CH2:19][CH:20]=[CH:21][c:22]1[cH:23][cH:24][c:25]([Cl:26])[cH:27][cH:28]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([O:12][CH3:13])[c:14]([F:15])[cH:16]...
COC(=O)c1cc(-c2ccc(OC)c(F)c2)n[nH]c1=O.ClCC=Cc1ccc(Cl)cc1
COC(=O)c1cc(-c2ccc(OC)c(F)c2)nn(CC=Cc2ccc(Cl)cc2)c1=O
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
456217c8bdd4490079dbc0339e1b1eedc560d0b24ec9d54c4ed1fbd8e71fb3dc
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=c1ccc(-c2ccccc2)nn1CC=Cc1ccccc1
Cl-[CH2;D2;+0:1]-[C:2]=[C:3]-[c:4].[#8:5]-[C:6](=[O;D1;H0:7])-[c:8]:[c:9](=[O;D1;H0:10]):[nH;D2;+0:11]:[#7;a:12]:[c:13]>>[#8:5]-[C:6](=[O;D1;H0:7])-[c:8]:[c:9](=[O;D1;H0:10]):[n;H0;D3;+0:11](-[CH2;D2;+0:1]-[C:2]=[C:3]-[c:4]):[#7;a:12]:[c:13]
51.1
[{"value": 51.1, "product": "ClC1=CC=C(C=CCN2N=C(C=C(C2=O)C(=O)OC)C2=CC(=C(C=C2)OC)F)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (6), 6-(3-fluoro-4-methoxyphenyl)-4-methoxycarbonyl-2H-pyridazin-3-one and 4-chlorocinnamyl chloride were reacted to yield the title compound as a pale yellow crystalline powder (yield: 51.1%). Conditions: See reaction.notes.procedure_details. Workup: were reacted
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1cnncc1
c1ccnnc1
c1ccnnc1.c1ccccc1.c1ccccc1
HCl
null
null
null
COC(=O)c1cc(-c2ccc(OC)c(F)c2)n[nH]c1=O.ClCC=Cc1ccc(Cl)cc1>>COC(=O)c1cc(-c2ccc(OC)c(F)c2)nn(CC=Cc2ccc(Cl)cc2)c1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c3de29e6ed0e4d46a8fd09b899695f45
COC(=O)c1cc(-c2ccc(OC)c(F)c2)nn(CC=Cc2ccc(Cl)cc2)c1=O>>COc1ccc(-c2cc(C(=O)O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
FC1=C(C=CC(=C1)F)C=1C=C(C(N(N1)CC(C)C)=O)COS(=O)(=O)C.ClC1=CC=C(C=CCN2N=C(C=C(C2=O)C(=O)OC)C2=CC(=C(C=C2)OC)F)C=C1>>C(=O)(O)C=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC=CC1=CC=C(C=C1)Cl)=O
C[O:12][C:10]([c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:28]([F:29])[cH:27]2)[n:26][n:15]([CH2:16][CH:17]=[CH:18][c:19]2[cH:20][cH:21][c:22]([Cl:23])[cH:24][cH:25]2)[c:13]1=[O:14])=[O:11]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([C:10](=[O:11])[OH:12])[c:13](=[O:14])[n:15]([CH2:16][CH:17]...
COC(=O)c1cc(-c2ccc(OC)c(F)c2)nn(CC=Cc2ccc(Cl)cc2)c1=O
COc1ccc(-c2cc(C(=O)O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
null
null
null
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=c1ccc(-c2ccccc2)nn1CC=Cc1ccccc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4]:[c:5]:[#7;a:6]>>[#7;a:6]:[c:5]:[c:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
98.2
[{"value": 98.2, "product": "C(=O)(O)C=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC=CC1=CC=C(C=C1)Cl)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (7), 2-(4-chlorocinnamyl)-6-(3-fluoro-4-methoxyphenyl)-4-methoxycarbonyl-2H-pyridazin-3-one was reacted to yield the title compound as a pale yellow crystalline powder (yield: 98.2%). Conditions: See reaction.notes.procedure_details. Workup: was reacted
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccnnc1.c1ccccc1
Other
null
null
null
COC(=O)c1cc(-c2ccc(OC)c(F)c2)nn(CC=Cc2ccc(Cl)cc2)c1=O>>COc1ccc(-c2cc(C(=O)O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ae51cee905cc4e5dbff0cb5b0ddd22c4
COc1ccc(-c2cc(C(=O)O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F>>COc1ccc(-c2cc(CO)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
FC1=C(C=CC(=C1)F)C=1C=C(C(N(N1)CC(C)C)=O)CN1C(C=2C(C1=O)=CC=CC2)=O.C(=O)(O)C=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC=CC1=CC=C(C=C1)Cl)=O>>ClC1=CC=C(C=CCN2N=C(C=C(C2=O)CO)C2=CC(=C(C=C2)OC)F)C=C1
O=[C:10]([c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:27]([F:28])[cH:26]2)[n:25][n:14]([CH2:15][CH:16]=[CH:17][c:18]2[cH:19][cH:20][c:21]([Cl:22])[cH:23][cH:24]2)[c:12]1=[O:13])[OH:11]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:10][OH:11])[c:12](=[O:13])[n:14]([CH2:15][CH:16]=[CH:17][c:1...
COc1ccc(-c2cc(C(=O)O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
COc1ccc(-c2cc(CO)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
null
null
null
Reduction
Reduction of carboxylic acid to primary alcohol
0db83a5ebe1e318b78b55461cf7eb8f7c004eef0f9e3b6666d3df4c96b5f665e
93b4621647b04d2ad2f2825215b1567f171ba61fe10d136b5db6ea0470aa4932
O=c1ccc(-c2ccccc2)nn1CC=Cc1ccccc1
O=[C;H0;D3;+0:1](-[O;D1;H1:2])-[c:3]1:[c:4]:[c:5]:[#7;a:6]:[#7;a:7](-[C:8]-[C:9]=[C:10]):[c:11]:1=[O;D1;H0:12]>>[C:10]=[C:9]-[C:8]-[#7;a:7]1:[#7;a:6]:[c:5]:[c:4]:[c:3](-[CH2;D2;+0:1]-[O;D1;H1:2]):[c:11]:1=[O;D1;H0:12]
17
[{"value": 17.0, "product": "ClC1=CC=C(C=CCN2N=C(C=C(C2=O)CO)C2=CC(=C(C=C2)OC)F)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (8), 4-carboxy-2-(4-chlorocinnamyl)-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one was reacted to yield the title compound as pale yellow crystals (yield: 17.0%). Conditions: See reaction.notes.procedure_details. Workup: was reacted
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary alcohol
null
null
c1ccccc1.c1ccnnc1.c1ccccc1
Other
null
null
null
COc1ccc(-c2cc(C(=O)O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F>>COc1ccc(-c2cc(CO)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0cb6dbb54fcd4d7bbc4967067b9d59ea
CN1CCNCC1.COc1ccc(-c2cc(COS(C)(=O)=O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F>>COc1ccc(-c2cc(CN3CCN(C)CC3)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
C(C)(C)(C)OC(=O)N1CCN(CC1)C=1C(N(N=C(C1C)C1=CC(=C(C=C1)C)F)CC(C)C)=O.ClC1=CC=C(C=CCN2N=C(C=C(C2=O)COS(=O)(=O)C)C2=CC(=C(C=C2)OC)F)C=C1.CN1CCNCC1>>ClC1=CC=C(C=CCN2N=C(C=C(C2=O)CN2CCN(CC2)C)C2=CC(=C(C=C2)OC)F)C=C1
[NH:11]1[CH2:12][CH2:13][N:14]([CH3:15])[CH2:16][CH2:17]1.CS(=O)(=O)O[CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:33]([F:34])[cH:32]2)[n:31][n:20]([CH2:21][CH:22]=[CH:23][c:24]2[cH:25][cH:26][c:27]([Cl:28])[cH:29][cH:30]2)[c:18]1=[O:19]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:...
CN1CCNCC1.COc1ccc(-c2cc(COS(C)(=O)=O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
COc1ccc(-c2cc(CN3CCN(C)CC3)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
bc40e881c80f733cc18ae6a4c32c0d2e3ac9ce7b07d3a2cb609684e869dc6007
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=c1c(CN2CCNCC2)cc(-c2ccccc2)nn1CC=Cc1ccccc1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[#7;a:6](-[C:7]-[C:8]=[C:9]):[c:10]:1=[O;D1;H0:11].[#7:12]1-[C:13]-[C:14]-[NH;D2;+0:15]-[C:16]-[C:17]-1>>[C:9]=[C:8]-[C:7]-[#7;a:6]1:[#7;a:5]:[c:4]:[c:3]:[c:2](-[CH2;D2;+0:1]-[N;H0;D3;+0:15]2-[C:14]-[C:13]-[#7:12]-[C:17]-[C:16]-2):[c:10]:1=[O;D1;H0:11]
66.3
[{"value": 66.3, "product": "ClC1=CC=C(C=CCN2N=C(C=C(C2=O)CN2CCN(CC2)C)C2=CC(=C(C=C2)OC)F)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (10), 2-(4-chlorocinnamyl)-6-(3-fluoro-4-methoxyphenyl)-4-methanesulfonyloxymethyl-2H-pyridazin-3-one and 1-methylpiperazine were reacted to yield the title compound as pale brown neeldes (yield: 66.3%). Conditions: See reaction.notes.procedure_details. Workup: were reacted
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
C1CNCC[NH]1
C1C[NH]CC[NH]1
c1ccccc1.c1ccnnc1.C1C[NH]CC[NH]1.c1ccccc1
MsOH.HO-
null
null
null
CN1CCNCC1.COc1ccc(-c2cc(COS(C)(=O)=O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F>>COc1ccc(-c2cc(CN3CCN(C)CC3)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-05e673c9e6fa437aa9ab215ba6dafd87
COc1ccc(-c2cc(COS(C)(=O)=O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F.OCCN1CCNCC1>>COc1ccc(-c2cc(CN3CCN(CCO)CC3)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
C(C)(C)(C)OC(=O)N1CCN(CC1)C=1C(N(N=C(C1C)C1=CC(=C(C=C1)C)F)CC(C)C)=O.ClC1=CC=C(C=CCN2N=C(C=C(C2=O)COS(=O)(=O)C)C2=CC(=C(C=C2)OC)F)C=C1.N1(CCNCC1)CCO>>ClC1=CC=C(C=CCN2N=C(C=C(C2=O)CN2CCN(CC2)CCO)C2=CC(=C(C=C2)OC)F)C=C1
CS(=O)(=O)O[CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:35]([F:36])[cH:34]2)[n:33][n:22]([CH2:23][CH:24]=[CH:25][c:26]2[cH:27][cH:28][c:29]([Cl:30])[cH:31][cH:32]2)[c:20]1=[O:21].[NH:11]1[CH2:12][CH2:13][N:14]([CH2:15][CH2:16][OH:17])[CH2:18][CH2:19]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[c...
COc1ccc(-c2cc(COS(C)(=O)=O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F.OCCN1CCNCC1
COc1ccc(-c2cc(CN3CCN(CCO)CC3)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
bc40e881c80f733cc18ae6a4c32c0d2e3ac9ce7b07d3a2cb609684e869dc6007
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=c1c(CN2CCNCC2)cc(-c2ccccc2)nn1CC=Cc1ccccc1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[#7;a:6](-[C:7]-[C:8]=[C:9]):[c:10]:1=[O;D1;H0:11].[#7:12]1-[C:13]-[C:14]-[NH;D2;+0:15]-[C:16]-[C:17]-1>>[C:9]=[C:8]-[C:7]-[#7;a:6]1:[#7;a:5]:[c:4]:[c:3]:[c:2](-[CH2;D2;+0:1]-[N;H0;D3;+0:15]2-[C:14]-[C:13]-[#7:12]-[C:17]-[C:16]-2):[c:10]:1=[O;D1;H0:11]
65.1
[{"value": 65.1, "product": "ClC1=CC=C(C=CCN2N=C(C=C(C2=O)CN2CCN(CC2)CCO)C2=CC(=C(C=C2)OC)F)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (10), 2-(4-chlorocinnamyl)-6-(3-fluoro-4-methoxyphenyl)-4-methanesulfonyloxymethyl-2H-pyridazin-3-one and 1-piperazineethanol were reacted to yield the title compound as slightly-yellow needles (yield: 65.1%). Conditions: See reaction.notes.procedure_details. Workup: were reacted
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
C1CNCC[NH]1
C1C[NH]CC[NH]1
c1ccccc1.c1ccnnc1.C1C[NH]CC[NH]1.c1ccccc1
MsOH.HO-
null
null
null
COc1ccc(-c2cc(COS(C)(=O)=O)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F.OCCN1CCNCC1>>COc1ccc(-c2cc(CN3CCN(CCO)CC3)c(=O)n(CC=Cc3ccc(Cl)cc3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-75f5140c9d8a44fa82529fda053a0ac4
BrC(Br)(Br)Br.COc1ccc(-c2nn(C3CC3)c(=O)c(CO)c2C)cc1F>>COc1ccc(-c2cc(CBr)c(=O)n(CC3CC3)n2)cc1F
C1(CC1)N1N=C(C(=C(C1=O)CO)C)C1=CC(=C(C=C1)OC)F.C(Br)(Br)(Br)Br.N1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>BrCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O
BrC(Br)(Br)[Br:11].C[c:8]1[c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:21]([F:22])[cH:20]2)[n:19][n:14]([CH:15]2[CH2:16][CH2:18]2)[c:12](=[O:13])[c:9]1[CH2:10]O>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:10][Br:11])[c:12](=[O:13])[n:14]([CH2:15][CH:16]3[CH2:17][CH2:18]3)[n:19]2)[cH:20][c:21]1[F:22]
BrC(Br)(Br)Br.COc1ccc(-c2nn(C3CC3)c(=O)c(CO)c2C)cc1F
COc1ccc(-c2cc(CBr)c(=O)n(CC3CC3)n2)cc1F
null
null
O1CCCC1
Functional Group Interconversion
OtherReaction
8f3e4f5e5a276936e09935a7fd0012eeeeccce5c831ce314373f7a4dc04c316e
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
O=c1ccc(-c2ccccc2)nn1CC1CC1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].C-[c;H0;D3;+0:2]1:[c:3](-[c:4]):[#7;a:5]:[#7;a:6](-[CH;D3;+0:7]2-[CH2;D2;+0:8]-[CH2;D2;+0:9]-2):[c:10](=[O;D1;H0:11]):[c:12]:1-[CH2;D2;+0:13]-O>>[Br;H0;D1;+0:1]-[CH2;D2;+0:13]-[c:12]1:[cH;D2;+0:2]:[c:3](-[c:4]):[#7;a:5]:[#7;a:6](-[CH2;D2;+0:7]-[CH;D3;+0:8]2-[C:14]-[CH2;D2;+0:9]-2):[c:10]:...
69.5
[{"value": 69.5, "product": "BrCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 69.2, "product": "BrCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
2-Cyclopropyl-methyl-6-(3-fluoro-4-methoxyphenyl)-4-hydroxymethyl-2H-pyridazin-3-one (185 mg, 0.61 mmol), carbon tetrabromide (404 mg, 1.2 mmol) and pyridine (48 mg, 0.61 mmol) were dissolved in tetrahydrofuran (3 mL), and under ice-cold stirring, a solution of triphenylphosphine (319 mg, 1.2 mmol) in tetrahydrofuran (...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
c1ccnnc1.C1CC1
c1ccnnc1.C1CC1
c1ccccc1.c1ccnnc1.C1CC1
HBr
O1CCCC1
null
1
BrC(Br)(Br)Br.COc1ccc(-c2nn(C3CC3)c(=O)c(CO)c2C)cc1F>O1CCCC1>COc1ccc(-c2cc(CBr)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-64b894aee23246cebcc958882c411997
CC(C)(C)OC(=O)CC(=O)OC(C)(C)C.COc1ccc(-c2cc(CBr)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(=O)n(CC3CC3)n2)cc1F
O.[H-].[Na+].C(CC(=O)OC(C)(C)C)(=O)OC(C)(C)C.BrCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O>>C1(CC1)CN1N=C(C=C(C1=O)CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C1=CC(=C(C=C1)OC)F
[CH2:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25].Br[CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:35]([F:36])[cH:34]2)[n:33][n:28]([CH2:29][CH:30]2[CH2:31][CH2:32]2)[c:26]1=[O:27]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:...
CC(C)(C)OC(=O)CC(=O)OC(C)(C)C.COc1ccc(-c2cc(CBr)c(=O)n(CC3CC3)n2)cc1F
COc1ccc(-c2cc(CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(=O)n(CC3CC3)n2)cc1F
null
null
CN(C=O)C
C-C Coupling
OtherReaction
8175b6573d6439ec7ccc45bf6b48843ab56b46dccfc6504384c4766d09f35cc7
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
O=c1ccc(-c2ccccc2)nn1CC1CC1
Br-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[#7;a:6](-[C:7]):[c:8]:1=[O;D1;H0:9].[C;D1;H3:10]-[C:11](-[C;D1;H3:12])(-[C;D1;H3:13])-[#8:14]-[C:15](=[O;D1;H0:16])-[CH2;D2;+0:17]-[C:18](=[O;D1;H0:19])-[#8:20]-[C:21](-[C;D1;H3:22])(-[C;D1;H3:23])-[C;D1;H3:24]>>[C:7]-[#7;a:6]1:[#7;a:5]:[c:4]:[c:3]:[c:2](-[CH2;D2;+0:1]-[CH;...
61.8
[{"value": 61.8, "product": "C1(CC1)CN1N=C(C=C(C1=O)CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C1=CC(=C(C=C1)OC)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 0.1, "product": "C1(CC1)CN1N=C(C=C(C1=O)CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C1=CC(=C(C=C1)OC)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
After 55% sodium hydride (322 mg, 7.38 mmol) was added to a solution of di-tert-butyl malonate (970 mg, 4.48 mmol) in N,N-dimethylformamide (10 mL), 4-bromomethyl-2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one (1.8 g, 4.90 mmol) was added under ice-cold stirring. The reaction mixture was stirred at...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
null
null
c1ccccc1.c1ccnnc1.C1CC1
HBr
CN(C=O)C
null
1
CC(C)(C)OC(=O)CC(=O)OC(C)(C)C.COc1ccc(-c2cc(CBr)c(=O)n(CC3CC3)n2)cc1F>CN(C=O)C>COc1ccc(-c2cc(CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-acc6327e872d44b5954e4f6a3294ed3c
COc1ccc(-c2cc(CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCC(=O)O)c(=O)n(CC3CC3)n2)cc1F
FC(C(=O)O)(F)F.C1(CC1)CN1N=C(C=C(C1=O)CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C1=CC(=C(C=C1)OC)F>>C(=O)(O)CCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O
CC(C)(C)OC(=O)[CH:11]([CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:24]([F:25])[cH:23]2)[n:22][n:17]([CH2:18][CH:19]2[CH2:20][CH2:21]2)[c:15]1=[O:16])[C:12](=[O:13])[O:14]C(C)(C)C>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:10][CH2:11][C:12](=[O:13])[OH:14])[c:15](=[O:16])[n:17]([C...
COc1ccc(-c2cc(CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(=O)n(CC3CC3)n2)cc1F
COc1ccc(-c2cc(CCC(=O)O)c(=O)n(CC3CC3)n2)cc1F
null
null
null
Reduction
OtherReaction
73d165f371e7be9e7ac8a17da558f54492bf9b0746a90d7cc3220d78efbe0c09
60f3a79f391ea73b07965c28fa39ab5eb6558d5e98c32a693ba93254730088b7
O=c1ccc(-c2ccccc2)nn1CC1CC1
C-C(-C)(-C)-O-C(=O)-[CH;D3;+0:1](-[C:2]-[c:3]:[c:4]:[#7;a:5])-[C:6](=[O;D1;H0:7])-[O;H0;D2;+0:8]-C(-C)(-C)-C>>[#7;a:5]:[c:4]:[c:3]-[C:2]-[CH2;D2;+0:1]-[C:6](=[O;D1;H0:7])-[OH;D1;+0:8]
94.7
[{"value": 94.7, "product": "C(=O)(O)CCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 94.5, "product": "C(=O)(O)CCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Trifluoroacetic acid (21 mL) was added to 2-cyclopropylmethyl-4-[2,2-di(tert-butoxycarbonyl)ethyl]-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one (1.39 g, 2.77 mmol), and the mixture was stirred at room temperature for 30 minutes. The solvent was distilled off under reduced pressure, and toluene was added further, fol...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Boc.Boc
Carboxylic acid
null
null
c1ccccc1.c1ccnnc1.C1CC1
HO-
null
null
0.5
COc1ccc(-c2cc(CC(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCC(=O)O)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cb5e1d7ad4974c3aabb1630f8ff71cea
COc1ccc(-c2cc(CCC(=O)O)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCO)c(=O)n(CC3CC3)n2)cc1F
FC1=C(C=CC(=C1)F)C=1C=C(C(N(N1)CC(C)C)=O)CN1C(C=2C(C1=O)=CC=CC2)=O.C(=O)(O)CCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O>>C1(CC1)CN1N=C(C=C(C1=O)CCCO)C1=CC(=C(C=C1)OC)F
O=[C:12]([CH2:11][CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:23]([F:24])[cH:22]2)[n:21][n:16]([CH2:17][CH:18]2[CH2:19][CH2:20]2)[c:14]1=[O:15])[OH:13]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:10][CH2:11][CH2:12][OH:13])[c:14](=[O:15])[n:16]([CH2:17][CH:18]3[CH2:19][CH2:20]3)[n...
COc1ccc(-c2cc(CCC(=O)O)c(=O)n(CC3CC3)n2)cc1F
COc1ccc(-c2cc(CCCO)c(=O)n(CC3CC3)n2)cc1F
null
null
null
Reduction
Reduction of carboxylic acid to primary alcohol
0db83a5ebe1e318b78b55461cf7eb8f7c004eef0f9e3b6666d3df4c96b5f665e
93b4621647b04d2ad2f2825215b1567f171ba61fe10d136b5db6ea0470aa4932
O=c1ccc(-c2ccccc2)nn1CC1CC1
O=[C;H0;D3;+0:1](-[O;D1;H1:2])-[C:3]-[C:4]>>[C:4]-[C:3]-[CH2;D2;+0:1]-[O;D1;H1:2]
82.9
[{"value": 82.9, "product": "C1(CC1)CN1N=C(C=C(C1=O)CCCO)C1=CC(=C(C=C1)OC)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (8), 4-(2-carboxyethyl)-2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one was reacted to yield the title compound as a brown oil (yield: 82.9%). Conditions: See reaction.notes.procedure_details. Workup: was reacted
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary alcohol
null
null
c1ccccc1.c1ccnnc1.C1CC1
Other
null
null
null
COc1ccc(-c2cc(CCC(=O)O)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCO)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e5bf283c17274c55acf4bfd501a63d4b
CN1CCNCC1.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCN3CCN(C)CC3)c(=O)n(CC3CC3)n2)cc1F
C(C)(C)(C)OC(=O)N1CCN(CC1)C=1C(N(N=C(C1C)C1=CC(=C(C=C1)C)F)CC(C)C)=O.C1(CC1)CN1N=C(C=C(C1=O)CCCOS(=O)(=O)C)C1=CC(=C(C=C1)OC)F.CN1CCNCC1>>C1(CC1)CN1N=C(C=C(C1=O)CCCN1CCN(CC1)C)C1=CC(=C(C=C1)OC)F
[NH:13]1[CH2:14][CH2:15][N:16]([CH3:17])[CH2:18][CH2:19]1.CS(=O)(=O)O[CH2:12][CH2:11][CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:29]([F:30])[cH:28]2)[n:27][n:22]([CH2:23][CH:24]2[CH2:25][CH2:26]2)[c:20]1=[O:21]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:10][CH2:11][CH2:12][N:13]...
CN1CCNCC1.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F
COc1ccc(-c2cc(CCCN3CCN(C)CC3)c(=O)n(CC3CC3)n2)cc1F
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
bc40e881c80f733cc18ae6a4c32c0d2e3ac9ce7b07d3a2cb609684e869dc6007
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=c1c(CCCN2CCNCC2)cc(-c2ccccc2)nn1CC1CC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[C:3].[#7:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[#7:4]-[C:9]-[C:8]-1
62
[{"value": 62.0, "product": "C1(CC1)CN1N=C(C=C(C1=O)CCCN1CCN(CC1)C)C1=CC(=C(C=C1)OC)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (10), 2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-4-(3-methanesulfonyloxypropyl)-2H-pyridazin-3-one and 1-methylpiperazine were reacted to yield the title compound as a yellow oil (yield: 62.0%). Conditions: See reaction.notes.procedure_details. Workup: were reacted
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
C1CNCC[NH]1
C1C[NH]CC[NH]1
c1ccccc1.c1ccnnc1.C1C[NH]CC[NH]1.C1CC1
MsOH.HO-
null
null
null
CN1CCNCC1.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCN3CCN(C)CC3)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3168b7d94c754219aa02a878634ae871
CNC.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCN(C)C)c(=O)n(CC3CC3)n2)cc1F
C1(CC1)CN1N=C(C=C(C1=O)CCCOS(=O)(=O)C)C1=CC(=C(C=C1)OC)F.CNC>>C1(CC1)CN1N=C(C=C(C1=O)CCCN(C)C)C1=CC(=C(C=C1)OC)F
[NH:13]([CH3:14])[CH3:15].CS(=O)(=O)O[CH2:12][CH2:11][CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:25]([F:26])[cH:24]2)[n:23][n:18]([CH2:19][CH:20]2[CH2:21][CH2:22]2)[c:16]1=[O:17]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:10][CH2:11][CH2:12][N:13]([CH3:14])[CH3:15])[c:16](=[O:17...
CNC.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F
COc1ccc(-c2cc(CCCN(C)C)c(=O)n(CC3CC3)n2)cc1F
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
ba24696731c43f94422863463da0ee528bfb8ec715fd228fe0a6c2ae67b49c25
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=c1ccc(-c2ccccc2)nn1CC1CC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[C:3].[C;D1;H3:4]-[NH;D2;+0:5]-[C;D1;H3:6]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:5](-[C;D1;H3:4])-[C;D1;H3:6]
64.7
[{"value": 64.7, "product": "C1(CC1)CN1N=C(C=C(C1=O)CCCN(C)C)C1=CC(=C(C=C1)OC)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 7, 2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-4-(3-methanesulfonyloxypropyl)-2H-pyridazin-3-one and dimethylamine were reacted to yield the title compound as a yellow powder (yield: 64.7%). Conditions: See reaction.notes.procedure_details. Workup: were reacted
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
null
null
c1ccccc1.c1ccnnc1.C1CC1
MsOH.HO-
null
null
null
CNC.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCN(C)C)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ef49fa90d7724a8e96e40b5cbe4b435d
CC(C)(C)OC(=O)N1CCNCC1.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCN3CCN(C(=O)OC(C)(C)C)CC3)c(=O)n(CC3CC3)n2)cc1F
C(C)(C)(C)OC(=O)N1CCN(CC1)C=1C(N(N=C(C1C)C1=CC(=C(C=C1)C)F)CC(C)C)=O.C1(CC1)CN1N=C(C=C(C1=O)CCCOS(=O)(=O)C)C1=CC(=C(C=C1)OC)F.N1(CCNCC1)C(=O)OC(C)(C)C>>C1(CC1)CN1N=C(C=C(C1=O)CCCN1CCN(CC1)C(=O)OC(C)(C)C)C1=CC(=C(C=C1)OC)F
[NH:13]1[CH2:14][CH2:15][N:16]([C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[CH2:24][CH2:25]1.CS(=O)(=O)O[CH2:12][CH2:11][CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:35]([F:36])[cH:34]2)[n:33][n:28]([CH2:29][CH:30]2[CH2:31][CH2:32]2)[c:26]1=[O:27]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[...
CC(C)(C)OC(=O)N1CCNCC1.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F
COc1ccc(-c2cc(CCCN3CCN(C(=O)OC(C)(C)C)CC3)c(=O)n(CC3CC3)n2)cc1F
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
bc40e881c80f733cc18ae6a4c32c0d2e3ac9ce7b07d3a2cb609684e869dc6007
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=c1c(CCCN2CCNCC2)cc(-c2ccccc2)nn1CC1CC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[C:3].[#7:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[#7:4]-[C:9]-[C:8]-1
76.9
[{"value": 76.9, "product": "C1(CC1)CN1N=C(C=C(C1=O)CCCN1CCN(CC1)C(=O)OC(C)(C)C)C1=CC(=C(C=C1)OC)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (10), 2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-4-(3-methanesulfonyloxypropyl)-2H-pyridazin-3-one and tert-butyl 1-piperazinecarboxylate were reacted to yield the title compound as a yellow oil (yield: 76.9%). Conditions: See reaction.notes.procedure_details. Workup: were rea...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
C1CNCC[NH]1
C1C[NH]CC[NH]1
c1ccccc1.c1ccnnc1.C1C[NH]CC[NH]1.C1CC1
MsOH.HO-
null
null
null
CC(C)(C)OC(=O)N1CCNCC1.COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCN3CCN(C(=O)OC(C)(C)C)CC3)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e4e0517e1a0e432fb39f25650571d446
COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F.OCCNCCO>>COc1ccc(-c2cc(CCCN(CCO)CCO)c(=O)n(CC3CC3)n2)cc1F
C(C)(C)(C)OC(=O)N1CCN(CC1)C=1C(N(N=C(C1C)C1=CC(=C(C=C1)C)F)CC(C)C)=O.C1(CC1)CN1N=C(C=C(C1=O)CCCOS(=O)(=O)C)C1=CC(=C(C=C1)OC)F.N(CCO)CCO>>OCCN(CCO)CCCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O
CS(=O)(=O)O[CH2:12][CH2:11][CH2:10][c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:29]([F:30])[cH:28]2)[n:27][n:22]([CH2:23][CH:24]2[CH2:25][CH2:26]2)[c:20]1=[O:21].[NH:13]([CH2:14][CH2:15][OH:16])[CH2:17][CH2:18][OH:19]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:10][CH2:11][CH2:12][N:13]([...
COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F.OCCNCCO
COc1ccc(-c2cc(CCCN(CCO)CCO)c(=O)n(CC3CC3)n2)cc1F
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
ba24696731c43f94422863463da0ee528bfb8ec715fd228fe0a6c2ae67b49c25
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
O=c1ccc(-c2ccccc2)nn1CC1CC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:6](-[C:5]-[C:4])-[C:7]-[C:8]
13.1
[{"value": 13.1, "product": "OCCN(CCO)CCCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 1 (10), 2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-4-(3-methanesulfonyloxypropyl)-2H-pyridazin-3-one and diethanolamine were reacted to yield the title compound as a yellow oil (yield: 13.1%). Conditions: See reaction.notes.procedure_details. Workup: were reacted
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
null
null
c1ccccc1.c1ccnnc1.C1CC1
MsOH.HO-
null
null
null
COc1ccc(-c2cc(CCCOS(C)(=O)=O)c(=O)n(CC3CC3)n2)cc1F.OCCNCCO>>COc1ccc(-c2cc(CCCN(CCO)CCO)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b29c56e897174da09d88d654baf61f7f
COc1ccc(-c2cc(CCCN3CCN(C(=O)OC(C)(C)C)CC3)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCN)c(=O)n(CC3CC3)n2)cc1F
C1(CC1)CN1N=C(C=C(C1=O)CCCN1CCN(CC1)C(=O)OC(C)(C)C)C1=CC(=C(C=C1)OC)F.C1(CC1)CN1N=C(C=C(C1=O)CCCOS(=O)(=O)C)C1=CC(=C(C=C1)OC)F>>NCCCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O
CC(C)(C)OC(=O)N1CC[N:13]([CH2:12][CH2:11][CH2:10][c:9]2[cH:8][c:7](-[c:6]3[cH:5][cH:4][c:3]([O:2][CH3:1])[c:23]([F:24])[cH:22]3)[n:21][n:16]([CH2:17][CH:18]3[CH2:19][CH2:20]3)[c:14]2=[O:15])CC1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([CH2:10][CH2:11][CH2:12][NH2:13])[c:14](=[O:15])[n:16]([CH2:17][CH:18]...
COc1ccc(-c2cc(CCCN3CCN(C(=O)OC(C)(C)C)CC3)c(=O)n(CC3CC3)n2)cc1F
COc1ccc(-c2cc(CCCN)c(=O)n(CC3CC3)n2)cc1F
null
null
null
Reduction
OtherReaction
23146a52518addfb1c2672d9eda28be46306c0529900b58e4e443b48598a246d
8db4ab69acf74a26aa2337e69e043c35d4e223d9c589e65301835fe886fa6f52
O=c1ccc(-c2ccccc2)nn1CC1CC1
C-C(-C)(-C)-O-C(=O)-N1-C-C-[N;H0;D3;+0:1](-[C:2]-[C:3])-C-C-1>>[C:3]-[C:2]-[NH2;D1;+0:1]
67.8
[{"value": 67.8, "product": "NCCCC=1C(N(N=C(C1)C1=CC(=C(C=C1)OC)F)CC1CC1)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 24 (1), 2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-4-(3-methanesulfonyloxypropyl)-2H-pyridazin-3-one was reacted to yield a crude product. Without purification, the crude product was reacted further in accordance with the procedure of Example 24 (2) to yield the title compound a...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Tertiary amine.Boc
Primary amine
C1CNCC[NH]1
null
c1ccccc1.c1ccnnc1.C1CC1
HO-
null
null
null
COc1ccc(-c2cc(CCCN3CCN(C(=O)OC(C)(C)C)CC3)c(=O)n(CC3CC3)n2)cc1F>>COc1ccc(-c2cc(CCCN)c(=O)n(CC3CC3)n2)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-178d1c80d262496d81b1b38dcd50183e
CC(C)CBr.N#Cc1ccc(O)cc1>>CC(C)COc1ccc(C#N)cc1
C(C(C)C)Br.C(#N)C1=CC=C(C=C1)O.C(C)N(CC)CC>>C(C(C)C)OC1=CC=C(C#N)C=C1
Br[CH2:4][CH:2]([CH3:1])[CH3:3].[OH:5][c:6]1[cH:7][cH:8][c:9]([C:10]#[N:11])[cH:12][cH:13]1>>[CH3:1][CH:2]([CH3:3])[CH2:4][O:5][c:6]1[cH:7][cH:8][c:9]([C:10]#[N:11])[cH:12][cH:13]1
CC(C)CBr.N#Cc1ccc(O)cc1
CC(C)COc1ccc(C#N)cc1
null
null
O.CN(C)C=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccccc1
Br-[CH2;D2;+0:1]-[C:2](-[C;D1;H3:3])-[C;D1;H3:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[C;D1;H3:3]-[C:2](-[C;D1;H3:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]
85.6
[{"value": 85.0, "product": "C(C(C)C)OC1=CC=C(C#N)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 85.6, "product": "C(C(C)C)OC1=CC=C(C#N)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
6
HOUR
To a solution of 4-cyanophenol (1.2 g, 10 mmol) in dry DMF (20 mL) was added triethylamine (20 mmol) followed by i-butyl bromide (2.7 g, 20 mmol). The resulting reaction mixture was stirred at 100° C. for 6 h. After cooling to room temperature, the reaction mixture was diluted with water (100 mL) and extracted with eth...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1
HBr
O.CN(C)C=O
100
6
CC(C)CBr.N#Cc1ccc(O)cc1>O.CN(C)C=O>CC(C)COc1ccc(C#N)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a2ee85c640ce4339a5e720ec558b5af4
CCN(CC)CCCO.O=[N+]([O-])c1cc(O)ccc1Cl>>CCN(CC)CCCOc1ccc(Cl)c([N+](=O)[O-])c1
ClC1=C(C=C(C=C1)O)[N+](=O)[O-].C(=O)([O-])[O-].[K+].[K+].CS(=O)(=O)Cl.C(C)N(CCCO)CC>>ClC1=C(C=C(C=C1)OCCCN(CC)CC)[N+](=O)[O-]
O[CH2:8][CH2:7][CH2:6][N:3]([CH2:2][CH3:1])[CH2:4][CH3:5].[OH:9][c:10]1[cH:11][cH:12][c:13]([Cl:14])[c:15]([N+:16](=[O:17])[O-:18])[cH:19]1>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][CH2:8][O:9][c:10]1[cH:11][cH:12][c:13]([Cl:14])[c:15]([N+:16](=[O:17])[O-:18])[cH:19]1
CCN(CC)CCCO.O=[N+]([O-])c1cc(O)ccc1Cl
CCN(CC)CCCOc1ccc(Cl)c([N+](=O)[O-])c1
null
null
CN(C)C=O.C(Cl)Cl
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether
86bfb73617450d22f9456ed5ce4d96a73f1f8fc0c016bebae57fda68e2da86a2
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccccc1
O-[CH2;D2;+0:1]-[C:2]-[C:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
90.7
[{"value": 90.7, "product": "ClC1=C(C=C(C=C1)OCCCN(CC)CC)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
MsCl (6.0 mmol) was added dropwise at 0° C. to a stirred solution of 3-diethylamino-1-propanol (6.0 mmol), TEA (6.0 mmol) in anhydrous DCM (6 mL), and the mixture was stirred at the same temperature for 10 min, and at room temperature for additional 1 h. After the removal of the solvent in vacuo, the solid residue was ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
null
c1ccccc1
HO-
CN(C)C=O.C(Cl)Cl
null
0.166667
CCN(CC)CCCO.O=[N+]([O-])c1cc(O)ccc1Cl>CN(C)C=O.C(Cl)Cl>CCN(CC)CCCOc1ccc(Cl)c([N+](=O)[O-])c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f375c00562a24af688c5e95063e27f6d
CCN(CC)CCCO.O=[N+]([O-])c1ccc(O)cc1F>>CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1
FC=1C=C(C=CC1[N+](=O)[O-])O.CS(=O)(=O)[O-].C(C)N(CCCO)CC.C(=O)([O-])[O-].[K+].[K+]>>FC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-]
O[CH2:8][CH2:7][CH2:6][N:3]([CH2:2][CH3:1])[CH2:4][CH3:5].[OH:9][c:10]1[cH:11][cH:12][c:13]([N+:14](=[O:15])[O-:16])[c:17]([F:18])[cH:19]1>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][CH2:8][O:9][c:10]1[cH:11][cH:12][c:13]([N+:14](=[O:15])[O-:16])[c:17]([F:18])[cH:19]1
CCN(CC)CCCO.O=[N+]([O-])c1ccc(O)cc1F
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether
86bfb73617450d22f9456ed5ce4d96a73f1f8fc0c016bebae57fda68e2da86a2
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccccc1
O-[CH2;D2;+0:1]-[C:2]-[C:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
null
[]
null
null
null
null
A solution of 3-fluoro-4-nitrophenol (2 mmol) and methanesulfonate of 3-diethylamino-1-propanol (2.5 mmol) in DMF (4 mL) is added with K2CO3 (4 mmol) and heated following the general procedure III (Step A). The product, 2-fluoro-4-(3-diethylamino-1-propoxy)nitrobenzene is obtained (470 mg) after purification using sili...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
null
c1ccccc1
HO-
CN(C)C=O
null
null
CCN(CC)CCCO.O=[N+]([O-])c1ccc(O)cc1F>CN(C)C=O>CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2376017b04d24493a40d98ac5b74b779
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1.[NH4+]>>CCN(CC)CCCOc1ccc([N+](=O)[O-])c(N)c1
FC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-].C([O-])([O-])=O.[NH4+].[NH4+].CCOC(=O)C>>[N+](=O)([O-])C1=C(N)C=C(C=C1)OCCCN(CC)CC
F[c:17]1[c:13]([N+:14](=[O:15])[O-:16])[cH:12][cH:11][c:10]([O:9][CH2:8][CH2:7][CH2:6][N:3]([CH2:2][CH3:1])[CH2:4][CH3:5])[cH:19]1.[NH4+:18]>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][CH2:8][O:9][c:10]1[cH:11][cH:12][c:13]([N+:14](=[O:15])[O-:16])[c:17]([NH2:18])[cH:19]1
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1.[NH4+]
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(N)c1
null
null
CN(C)C=O
Functional Group Interconversion
OtherReaction
0b3f36c6e96a844ac8c671a85ab317446ee29bfa735a32d39184f4616cac3a55
560c85d40afb1a57d77cf3258abf3be5bba829f35224f8687bf9a1d4c1f94bd9
c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[NH4+;D0:7]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH2;D1;+0:7]):[c:2]:[c:3]
null
[]
80
CELSIUS
null
null
The nitro compound obtained as above (1.5 mmol) is dissolved in DMF (4 mL) and added with ammonium carbonate (500 mg). The reaction mixture is then heated at 80° C. for 48 h. EtOAc (2×10 mL). The combined organic layers are then washed with water and brine and dried over Na2SO4. Removal of the solvent in vacuo yielded ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccccc1
c1ccccc1
c1ccccc1
HF
CN(C)C=O
80
null
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1.[NH4+]>CN(C)C=O>CCN(CC)CCCOc1ccc([N+](=O)[O-])c(N)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a53bb23cec524e1b93bdd268e5e66548
CCCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1>>CCCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
FC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-].C(CCC)N>>C(CCC)NC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-]
[CH3:1][CH2:2][CH2:3][CH2:4][NH2:5].F[c:6]1[cH:7][c:8]([O:9][CH2:10][CH2:11][CH2:12][N:13]([CH2:14][CH3:15])[CH2:16][CH3:17])[cH:18][cH:19][c:20]1[N+:21](=[O:22])[O-:23]>>[CH3:1][CH2:2][CH2:3][CH2:4][NH:5][c:6]1[cH:7][c:8]([O:9][CH2:10][CH2:11][CH2:12][N:13]([CH2:14][CH3:15])[CH2:16][CH3:17])[cH:18][cH:19][c:20]1[N+:21...
CCCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1
CCCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation primary amine
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:9]-[C:8]-[C:7]):[c:2]:[c:3]
null
[]
null
null
null
null
A solution of 2-fluoro-4-(3-diethylamino-1-propoxy)nitrobenzene (2 mmol; preparation described in Example 5) in THF (5 mL) is treated with n-butylamine (2.4 eq) at rt. After completion of the reaction, the reaction mixture is concentrated in vacuo. The residue is redissolved in EtOAc (10 mL), washed with saturated sodi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1
HF
C1CCOC1
null
null
CCCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1>C1CCOC1>CCCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a32838925aa044bb98e4a272dcdd9e10
CCN(CC)CCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1>>CCN(CC)CCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
FC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-].C(C)N(CCCN)CC>>C(C)N(CCCNC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-])CC
[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][CH2:8][NH2:9].F[c:10]1[cH:11][c:12]([O:13][CH2:14][CH2:15][CH2:16][N:17]([CH2:18][CH3:19])[CH2:20][CH3:21])[cH:22][cH:23][c:24]1[N+:25](=[O:26])[O-:27]>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][CH2:8][NH:9][c:10]1[cH:11][c:12]([O:13][CH2:14][CH2:15][CH2:16][N:1...
CCN(CC)CCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1
CCN(CC)CCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation primary amine
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:9]-[C:8]-[C:7]):[c:2]:[c:3]
null
[]
null
null
null
null
A solution of 2-fluoro-4-(3-diethylamino-1-propoxy)nitrobenzene (2 mmol; preparation described in Example 5) in THF (5 mL) is treated with 3-diethylamino-1-propylamine (2.4 mmol at rt. After completion of the reaction, the reaction mixture is concentrated in vacuo. The residue is redissolved in EtOAc (10 mL), washed wi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1
HF
C1CCOC1
null
null
CCN(CC)CCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1>C1CCOC1>CCN(CC)CCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8387d2f954384bf0b74112334218b3c6
CCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1>>CCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
FC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-].C(C)N>>C(C)NC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-]
[CH3:1][CH2:2][NH2:3].F[c:4]1[cH:5][c:6]([O:7][CH2:8][CH2:9][CH2:10][N:11]([CH2:12][CH3:13])[CH2:14][CH3:15])[cH:16][cH:17][c:18]1[N+:19](=[O:20])[O-:21]>>[CH3:1][CH2:2][NH:3][c:4]1[cH:5][c:6]([O:7][CH2:8][CH2:9][CH2:10][N:11]([CH2:12][CH3:13])[CH2:14][CH3:15])[cH:16][cH:17][c:18]1[N+:19](=[O:20])[O-:21]
CCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1
CCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation primary amine
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C;D1;H3:7]-[C:8]-[NH2;D1;+0:9]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:9]-[C:8]-[C;D1;H3:7]):[c:2]:[c:3]
88
[{"value": 88.0, "product": "C(C)NC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 2-fluoro-4-(3-diethylamino-1-propoxy)nitrobenzene (2 mmol; preparation described in Example 5) in THF (5 mL) is treated with ethylamine (4 mmol) at rt. After completion of the reaction, the reaction mixture is concentrated in vacuo. The residue is redissolved in EtOAc (10 mL), washed with saturated sodium...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1
HF
C1CCOC1
null
null
CCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1>C1CCOC1>CCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-af39e966e26540f5ac091befab22f4c6
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1.NCc1ccccc1>>CCN(CC)CCCOc1ccc([N+](=O)[O-])c(NCc2ccccc2)c1
FC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-].C(C1=CC=CC=C1)N>>C(C1=CC=CC=C1)NC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-]
F[c:17]1[c:13]([N+:14](=[O:15])[O-:16])[cH:12][cH:11][c:10]([O:9][CH2:8][CH2:7][CH2:6][N:3]([CH2:2][CH3:1])[CH2:4][CH3:5])[cH:26]1.[NH2:18][CH2:19][c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][CH2:8][O:9][c:10]1[cH:11][cH:12][c:13]([N+:14](=[O:15])[O-:16])[c:17]([NH:18][...
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1.NCc1ccccc1
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(NCc2ccccc2)c1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation primary amine
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(CNc2ccccc2)cc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[NH2;D1;+0:7]-[C:8]-[c:9]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:7]-[C:8]-[c:9]):[c:2]:[c:3]
86.7
[{"value": 86.7, "product": "C(C1=CC=CC=C1)NC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 2-fluoro-4-(3-diethylamino-1-propoxy)nitrobenzene (2 mmol; preparation described in Example 5) in THF (5 mL) is treated with benzylamine (2.4 mmol) at rt. After completion of the reaction, the reaction mixture is concentrated in vacuo. The residue is redissolved in EtOAc (10 mL), washed with saturated sod...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HF
C1CCOC1
null
null
CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1.NCc1ccccc1>C1CCOC1>CCN(CC)CCCOc1ccc([N+](=O)[O-])c(NCc2ccccc2)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d05a77cbb12a408ea3040c2e02249524
CCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1>>CCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
FC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-].C(CC)N>>C(CC)NC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-]
[CH3:1][CH2:2][CH2:3][NH2:4].F[c:5]1[cH:6][c:7]([O:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:13][CH3:14])[CH2:15][CH3:16])[cH:17][cH:18][c:19]1[N+:20](=[O:21])[O-:22]>>[CH3:1][CH2:2][CH2:3][NH:4][c:5]1[cH:6][c:7]([O:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:13][CH3:14])[CH2:15][CH3:16])[cH:17][cH:18][c:19]1[N+:20](=[O:21])[O-:22...
CCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1
CCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation primary amine
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:9]-[C:8]-[C:7]):[c:2]:[c:3]
87.3
[{"value": 87.3, "product": "C(CC)NC1=C(C=CC(=C1)OCCCN(CC)CC)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 2-fluoro-4-(3-diethylamino-1-propoxy)nitrobenzene (2 mmol; preparation described in Example 5) in THF (5 mL) is treated with propylamine (3 mmol) at rt. After completion of the reaction, the reaction mixture is concentrated in vacuo. The residue is redissolved in EtOAc (10 mL), washed with saturated sodiu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1
HF
C1CCOC1
null
null
CCCN.CCN(CC)CCCOc1ccc([N+](=O)[O-])c(F)c1>C1CCOC1>CCCNc1cc(OCCCN(CC)CC)ccc1[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6fe2fc3ae60d43a599678970974d3fca
NN.O=[N+]([O-])c1ccc(Cl)nc1>>NNc1ccc([N+](=O)[O-])cn1
ClC1=NC=C(C=C1)[N+](=O)[O-].O.NN>>[N+](=O)([O-])C=1C=CC(=NC1)NN
[NH2:1][NH2:2].Cl[c:3]1[cH:4][cH:5][c:6]([N+:7](=[O:8])[O-:9])[cH:10][n:11]1>>[NH2:1][NH:2][c:3]1[cH:4][cH:5][c:6]([N+:7](=[O:8])[O-:9])[cH:10][n:11]1
NN.O=[N+]([O-])c1ccc(Cl)nc1
NNc1ccc([N+](=O)[O-])cn1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
bbfd7563459ad1792ea1bdeb15b833ba71625ca5c9310b24f82e4f1a166d7f3e
61806bbf8bb8981e140ee503663af0ef0e69dc4f34f6582f974a2e4218f7da88
c1ccncc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5].[N;D1;H2:6]-[NH2;D1;+0:7]>>[N;D1;H2:6]-[NH;D2;+0:7]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
null
null
To a solution of 2-chloro-5-nitropyridine (30 mmol, 5.0 g) in absolute ethanol was added a solution of hydrazine hydrate (320 mmol, 15.8 g) in ethanol using syringe pump. At the end of the addition, the reaction was refrigerated. The named product precipitated from the reaction medium, was collected by filtration, and ...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Aromatic halide
Hydrazine
c1ccncc1
c1ccncc1
c1ccncc1
HCl
C(C)O
null
null
NN.O=[N+]([O-])c1ccc(Cl)nc1>C(C)O>NNc1ccc([N+](=O)[O-])cn1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e5691291fb0a4b04b21a9e9c660b0e4b
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccc(Br)cc1>>CCOC(=O)c1c(C)nn(-c2ccc(Br)cc2)c1C
Cl.BrC1=CC=C(C=C1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.C(Cl)(Cl)Cl>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC=C(C=C1)Br)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:18](=O)[CH3:19])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][c:14]([Br:15])[cH:16][cH:17]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][c:14]([Br:15])[cH:16][cH:17]2)[c:18]1[CH3:19]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccc(Br)cc1
CCOC(=O)c1c(C)nn(-c2ccc(Br)cc2)c1C
null
null
N1=CC=CC=C1.C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
8
HOUR
p-Bromophenylhydrazine hydrochloride (10 mmol, 2.5 g) was added to 2-acetyl-3-oxo-butyric acid ethyl ester (10 mmol, 1.7 g) in ethanol (10 mL) and pyridine (10 mL). The mixture was stirred overnight at room temperature. Thin layer chromatographic (TLC) analysis using chloroform indicated the reaction was complete. The ...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
N1=CC=CC=C1.C(C)O
null
8
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccc(Br)cc1>N1=CC=CC=C1.C(C)O>CCOC(=O)c1c(C)nn(-c2ccc(Br)cc2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-429914abd99c47c1b147ebf79f741665
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc([N+](=O)[O-])c1>>CCOC(=O)c1c(C)nn(-c2cccc([N+](=O)[O-])c2)c1C
Cl.[N+](=O)([O-])C=1C=C(C=CC1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC(=CC=C1)[N+](=O)[O-])C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:20](=O)[CH3:21])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][c:15]([N+:16](=[O:17])[O-:18])[cH:19]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][c:15]([N+:16](=[O:17])[O-:18])[cH:19]2)[c:20]1[CH3:21]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc([N+](=O)[O-])c1
CCOC(=O)c1c(C)nn(-c2cccc([N+](=O)[O-])c2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
null
null
Similar to Example 1, m-nitrophenylhydrazine hydrochloride (10 mmol, 1.9 g) and 2-acetyl-3-oxo-butyric acid ethyl ester (10 mmol, 1.7 g) were mixed in a 50% solution of pyridine in ethanol. A precipitate was formed in the reaction medium, and was collected by filtration. Analysis confirmed synthesis of the named produc...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc([N+](=O)[O-])c1>C(C)O>CCOC(=O)c1c(C)nn(-c2cccc([N+](=O)[O-])c2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-32740fb7cd88475c80964fc430e15578
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccc1>>CCOC(=O)c1c(C)nn(-c2ccccc2)c1C
C1(=CC=CC=C1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC=CC=C1)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:17](=O)[CH3:18])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[c:17]1[CH3:18]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccc1
CCOC(=O)c1c(C)nn(-c2ccccc2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
null
null
Similar to Example 1, phenyl hydrazine (7.5 mmol, 0.8 g) and 2-acetyl-3-oxo-butyric acid ethyl ester (7.5 mmol, 1.3 g) were mixed in a solution of 50% pyridine in ethanol. The solvents were removed under vacuum and the oil resuspended in chloroform. The resulting suspension was washed with 5% sodium bicarbonate, 5% hyd...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccc1>C(C)O>CCOC(=O)c1c(C)nn(-c2ccccc2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8a2a370daa1e478a88c3bf3e9f78a9ca
CCOC(=O)C(C(C)=O)C(C)=O.Cc1ccc(NN)cc1>>CCOC(=O)c1c(C)nn(-c2ccc(C)cc2)c1C
C1(=CC=C(C=C1)NN)C.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC=C(C=C1)C)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:18](=O)[CH3:19])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][c:14]([CH3:15])[cH:16][cH:17]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][c:14]([CH3:15])[cH:16][cH:17]2)[c:18]1[CH3:19]
CCOC(=O)C(C(C)=O)C(C)=O.Cc1ccc(NN)cc1
CCOC(=O)c1c(C)nn(-c2ccc(C)cc2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
null
null
Similar to Example 1, p-tolylhydrazine (10 mmol, 1.8 g) and 2-acetyl-3-oxo-butyric acid ethyl ester (10 mmol, 1.7 g) were mixed in a solution of 50% pyridine in ethanol. The solvents were removed under vacuum. The named product was purified over silica gel (m.p. 47° C.–49° C.). Conditions: See reaction.notes.procedure_...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.Cc1ccc(NN)cc1>C(C)O>CCOC(=O)c1c(C)nn(-c2ccc(C)cc2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ca83e3a45b8246e188eadb65c21b8275
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccc1[N+](=O)[O-]>>CCOC(=O)c1c(C)nn(-c2ccccc2[N+](=O)[O-])c1C
[N+](=O)([O-])C1=C(C=CC=C1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=C(C=CC=C1)[N+](=O)[O-])C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:20](=O)[CH3:21])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][c:16]1[N+:17](=[O:18])[O-:19]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[N+:17](=[O:18])[O-:19])[c:20]1[CH3:21]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccc1[N+](=O)[O-]
CCOC(=O)c1c(C)nn(-c2ccccc2[N+](=O)[O-])c1C
null
null
C(Cl)(Cl)Cl.CCCCCC.C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[#7;+:10]-[c:11](:[c:12]):[c;H0;D3;+0:13](-[NH;D2;+0:14]-[NH2;D1;+0:15]):[c:16]:[c:17]>>[#7;+:10]-[c:11](:[c:12]):[c;H0;D3;+0:13](-[n;H0;D3;+0:14]1:[n;H0;D2;+0:15]:[c;H0;D3;+0:8](-[C;D1;H3:9]):[c;H0;D3;+0:3](-[...
null
[]
null
null
null
null
Similar to Example 1, o-nitrophenylhydrazine (20 mmol, 3.4 g) and 2-acetyl-3-oxo-butyric acid ethyl ester (20 mmol, 3.4 g) were mixed in a solution of 50% pyridine in ethanol and heated under reflux. The solvents then were removed under vacuum, and the residue was resuspended in chloroform. The resulting mixture was wa...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(Cl)(Cl)Cl.CCCCCC.C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccc1[N+](=O)[O-]>C(Cl)(Cl)Cl.CCCCCC.C(C)O>CCOC(=O)c1c(C)nn(-c2ccccc2[N+](=O)[O-])c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ed62a267b1e1458b8a6848506377f05d
CCOC(=O)c1c(C)nn(-c2ccccc2[N+](=O)[O-])c1C>>CCOC(=O)c1c(C)nn(-c2ccccc2N)c1C
C(C)OC(=O)C=1C(=NN(C1C)C1=C(C=CC=C1)[N+](=O)[O-])C.C(C)O.[H][H]>>C(C)OC(=O)C=1C(=NN(C1C)C1=C(C=CC=C1)N)C
O=[N+:17]([O-])[c:16]1[c:11](-[n:10]2[n:9][c:7]([CH3:8])[c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:18]2[CH3:19])[cH:12][cH:13][cH:14][cH:15]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[NH2:17])[c:18]1[CH3:19]
CCOC(=O)c1c(C)nn(-c2ccccc2[N+](=O)[O-])c1C
CCOC(=O)c1c(C)nn(-c2ccccc2N)c1C
null
[Pd]
C(C)(=O)OCC
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(-n2cccn2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
To a solution of 3,5-dimethyl-1-(2-nitrophenyl)-1H-pyrazole-4-carboxylic acid ethyl ester (0.4 g) in a solution of equal proportions of ethanol and ethyl acetate was added 5% Pd/C (37 mg). The solution was treated with hydrogen gas at 45 psi. Upon completion of the reaction, the mixture was filtered through Celite, the...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1cn[nH]c1.c1ccccc1
Other
[Pd].C(C)(=O)OCC
null
null
CCOC(=O)c1c(C)nn(-c2ccccc2[N+](=O)[O-])c1C>[Pd].C(C)(=O)OCC>CCOC(=O)c1c(C)nn(-c2ccccc2N)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d66dcc09bc84436bab5835d34320f478
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccn1>>CCOC(=O)c1c(C)nn(-c2ccccn2)c1C
N1=C(C=CC=C1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=NC=CC=C1)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:17](=O)[CH3:18])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][n:16]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][cH:15][n:16]2)[c:17]1[CH3:18]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccn1
CCOC(=O)c1c(C)nn(-c2ccccn2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)nc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[#7;a:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[#7;a:13]:[c:14]):[...
null
[]
null
null
null
null
Similar to Example 1, 2-pyridylhydrazine (7.5 mmol, 0.8 g) and 2-acetyl-3-oxo-butyric acid ethyl ester (7.5 mmol, 1.3 g) were mixed in a solution of 50% pyridine in ethanol, then heated under reflux. The solvents were removed under vacuum and the residue purified over silica. The named product crystallized upon standin...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccncc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccccn1>C(C)O>CCOC(=O)c1c(C)nn(-c2ccccn2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7fc1f7aaa5b34943a693ad3861040cc8
CCOC(=O)c1c(C)nn(-c2cccc([N+](=O)[O-])c2)c1C>>CCOC(=O)c1c(C)nn(-c2cccc(N)c2)c1C
C(C)OC(=O)C=1C(=NN(C1C)C1=CC(=CC=C1)[N+](=O)[O-])C.[H][H]>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC(=CC=C1)N)C
O=[N+:16]([O-])[c:15]1[cH:14][cH:13][cH:12][c:11](-[n:10]2[n:9][c:7]([CH3:8])[c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:18]2[CH3:19])[cH:17]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][c:15]([NH2:16])[cH:17]2)[c:18]1[CH3:19]
CCOC(=O)c1c(C)nn(-c2cccc([N+](=O)[O-])c2)c1C
CCOC(=O)c1c(C)nn(-c2cccc(N)c2)c1C
null
[Pd]
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(-n2cccn2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
The compound of Example 2 (1.8 g) was dissolved in ethanol then 0.2 g 5% Pd/C was added to the solution. The mixture was treated with hydrogen gas at 45 psi. Upon completion of the reaction, the solution was filtered through Celite, and the filtrate concentrated under vacuum. The named product slowly crystallized upon ...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1cn[nH]c1.c1ccccc1
Other
[Pd].C(C)O
null
null
CCOC(=O)c1c(C)nn(-c2cccc([N+](=O)[O-])c2)c1C>[Pd].C(C)O>CCOC(=O)c1c(C)nn(-c2cccc(N)c2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3dfffe55f58b4bbcb2b5d2ddd09a9a2a
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccc([N+](=O)[O-])cn1>>CCOC(=O)c1c(C)nn(-c2ccc([N+](=O)[O-])cn2)c1C
[N+](=O)([O-])C=1C=CC(=NC1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=NC=C(C=C1)[N+](=O)[O-])C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:20](=O)[CH3:21])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][c:14]([N+:15](=[O:16])[O-:17])[cH:18][n:19]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][c:14]([N+:15](=[O:16])[O-:17])[cH:18][n:19]2)[c:20]1[CH3:21]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccc([N+](=O)[O-])cn1
CCOC(=O)c1c(C)nn(-c2ccc([N+](=O)[O-])cn2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)nc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[#7;a:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[#7;a:13]:[c:14]):[...
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of (5-nitropyridin-2-yl)hydrazine and 2-acetyl-3-oxo-butyric acid ethyl ester were combined in a solution of 50% pyridine in ethanol. Analysis confirmed synthesis of the named product (m.p. 117° C.–119° C.). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccncc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNc1ccc([N+](=O)[O-])cn1>C(C)O>CCOC(=O)c1c(C)nn(-c2ccc([N+](=O)[O-])cn2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-41bda36bf6214c4a9b8efca6708532c2
CCOC(=O)C(C(C)=O)C(C)=O.NNC1CCCCC1>>CCOC(=O)c1c(C)nn(C2CCCCC2)c1C
Cl.C1(CCCCC1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1CCCCC1)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:17](=O)[CH3:18])[CH3:8].[NH2:9][NH:10][CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10]([CH:11]2[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]2)[c:17]1[CH3:18]
CCOC(=O)C(C(C)=O)C(C)=O.NNC1CCCCC1
CCOC(=O)c1c(C)nn(C2CCCCC2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1cnn(C2CCCCC2)c1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[C:10]-[C:11](-[NH;D2;+0:12]-[NH2;D1;+0:13])-[C:14]>>[C:10]-[C:11](-[n;H0;D3;+0:12]1:[n;H0;D2;+0:13]:[c;H0;D3;+0:8](-[C;D1;H3:9]):[c;H0;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7]):[c;H0;D3;+0:1]:1-[C;D1;H3:2])-...
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of cyclohexyl hydrazine hydrochloride and 2-acetyl-3-oxobutyric acid ethyl ester were combined in a solution of 50% pyridine in ethanol. Analysis confirmed synthesis of the named product (m.p. 66° C.–67° C.). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.C1CCCCC1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNC1CCCCC1>C(C)O>CCOC(=O)c1c(C)nn(C2CCCCC2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cdce1d85350340c0aefc14ad614d2d49
CCOC(=O)C(C(C)=O)C(C)=O.NNCc1ccccc1>>CCOC(=O)c1c(C)nn(Cc2ccccc2)c1C
Cl.Cl.C(C1=CC=CC=C1)NN.N1=CC=CC=C1.C(C)OC(C(C(C)=O)C(C)=O)=O>>C(C)OC(=O)C=1C(=NN(C1C)CC1=CC=CC=C1)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:18](=O)[CH3:19])[CH3:8].[NH2:9][NH:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10]([CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[c:18]1[CH3:19]
CCOC(=O)C(C(C)=O)C(C)=O.NNCc1ccccc1
CCOC(=O)c1c(C)nn(Cc2ccccc2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(Cn2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[C:12]-[c:13]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[C:12]-[c:13]):[n;H0;D2;+0:10]:[c;H0;D3;+0:8]:1-[C;D1;H3:9]
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of benzylhydrazine dihydrochloride and 2-acetyl-3-oxo-butyric acid ethyl ester were combined in a solution of 50% pyridine in ethanol. The resulting oil was determined to be the named product by 1H-NMR (CDCl3, ppm): 1.35 t (3H); 2.44 s (3H); 2.45 s (3H); 4.38 a (2H); 5.25 s (2H);...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNCc1ccccc1>C(C)O>CCOC(=O)c1c(C)nn(Cc2ccccc2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c9ce789e8e2a4048869aacc55103453f
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(Cl)c1>>CCOC(=O)c1c(C)nn(-c2cccc(Cl)c2)c1C
Cl.ClC=1C=C(C=CC1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC(=CC=C1)Cl)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:18](=O)[CH3:19])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][c:15]([Cl:16])[cH:17]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][c:15]([Cl:16])[cH:17]2)[c:18]1[CH3:19]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(Cl)c1
CCOC(=O)c1c(C)nn(-c2cccc(Cl)c2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of 3-chlorophenylhydrazine hydrochloride and 2-acetyl-3-oxo-butyric acid ethyl ester were combined in a solution of 50% pyridine in ethanol. Analysis confirmed that the resulting solid was determined to be the named product (m.p. 56° C.–57° C.). Conditions: See reaction.notes.pro...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(Cl)c1>C(C)O>CCOC(=O)c1c(C)nn(-c2cccc(Cl)c2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-10ff9f3ebf424ef1bf07a369dc0fa429
CCOC(=O)C(C(C)=O)C(C)=O.Cc1cccc(NN)c1>>CCOC(=O)c1c(C)nn(-c2cccc(C)c2)c1C
Cl.C1(=CC(=CC=C1)NN)C.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C=1C=C(C=CC1)C)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:18](=O)[CH3:19])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][c:15]([CH3:16])[cH:17]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][c:15]([CH3:16])[cH:17]2)[c:18]1[CH3:19]
CCOC(=O)C(C(C)=O)C(C)=O.Cc1cccc(NN)c1
CCOC(=O)c1c(C)nn(-c2cccc(C)c2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of m-tolylhydrazine hydrochloride and 2-acetyl-3-oxo-butyric acid ethyl ester were combined in a solution of a 50% pyridine in ethanol. The resulting oil was purified by flash chromatography to yield the named product as a solid (m.p. 46.5° C.–47.5° C.). Conditions: See reaction....
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.Cc1cccc(NN)c1>C(C)O>CCOC(=O)c1c(C)nn(-c2cccc(C)c2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-50a50e2c29a64a198360ea13b9febfaf
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(F)c1>>CCOC(=O)c1c(C)nn(-c2cccc(F)c2)c1C
Cl.FC=1C=C(C=CC1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC(=CC=C1)F)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:18](=O)[CH3:19])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][c:15]([F:16])[cH:17]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][c:15]([F:16])[cH:17]2)[c:18]1[CH3:19]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(F)c1
CCOC(=O)c1c(C)nn(-c2cccc(F)c2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of 3-fluorophenylhydrazine hydrochloride and 2-acetyl-3-oxo-butyric acid ethyl ester were combined in a solution of 50% pyridine in ethanol. Analysis showed that resulting solid was the named product (m.p. 55° C.–56.1° C.). Conditions: See reaction.notes.procedure_details. Workup...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(F)c1>C(C)O>CCOC(=O)c1c(C)nn(-c2cccc(F)c2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6d47505205454e4dbf465abd74ce19e3
CCOC(=O)C(C(C)=O)C(C)=O.COc1cccc(NN)c1>>CCOC(=O)c1c(C)nn(-c2cccc(OC)c2)c1C
Cl.COC=1C=C(C=CC1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC(=CC=C1)OC)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:19](=O)[CH3:20])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][c:15]([O:16][CH3:17])[cH:18]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][c:15]([O:16][CH3:17])[cH:18]2)[c:19]1[CH3:20]
CCOC(=O)C(C(C)=O)C(C)=O.COc1cccc(NN)c1
CCOC(=O)c1c(C)nn(-c2cccc(OC)c2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of 3-methoxyphenylhydrazine hydrochloride and 2-acetyl-3-oxo-butyric acid ethyl ester were combined in a solution of 50% pyridine in ethanol. The resulting solid was determined to be the named product by 1H-NMR (CDCl3, ppm): 1.38 t (3H); 2.50 s (3H); 2.52 s (3H); 3.84 s (3H); 4.3...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.COc1cccc(NN)c1>C(C)O>CCOC(=O)c1c(C)nn(-c2cccc(OC)c2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-96e1a28570e240d998aab5642757c5ed
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(Br)c1>>CCOC(=O)c1c(C)nn(-c2cccc(Br)c2)c1C
Cl.BrC=1C=C(C=CC1)NN.C(C)OC(C(C(C)=O)C(C)=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1C)C1=CC(=CC=C1)Br)C
O=[C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:18](=O)[CH3:19])[CH3:8].[NH2:9][NH:10][c:11]1[cH:12][cH:13][cH:14][c:15]([Br:16])[cH:17]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH3:8])[n:9][n:10](-[c:11]2[cH:12][cH:13][cH:14][c:15]([Br:16])[cH:17]2)[c:18]1[CH3:19]
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(Br)c1
CCOC(=O)c1c(C)nn(-c2cccc(Br)c2)c1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
ab164a2f07e9367856bf3c71fa902c37bbb79de5ea024b32fa79526bb18dc4d6
7abcc9a477ed734c13c96188d72c44fdd5cc90ff2d36e50b359d7dc8b3f07d61
c1ccc(-n2cccn2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:3](-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7])-[C;H0;D3;+0:8](=O)-[C;D1;H3:9].[NH2;D1;+0:10]-[NH;D2;+0:11]-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:1](-[C;D1;H3:2]):[n;H0;D3;+0:11](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:...
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of 3-bromophenylhydrazine hydrochloride and 2-acetyl-3-oxo-butyric acid ethyl ester were combined in a solution of 50% pyridine in ethanol. Analysis showed that the resulting solid was the named product (m.p. 34° C.–35° C.). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1
HO-
C(C)O
null
null
CCOC(=O)C(C(C)=O)C(C)=O.NNc1cccc(Br)c1>C(C)O>CCOC(=O)c1c(C)nn(-c2cccc(Br)c2)c1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d784be3dc1194f6b9ccfbea658a1aa5c
CCOC(=O)C(C=O)C(C)=O.NNc1ccccn1>>CCOC(=O)c1cn(-c2ccccn2)nc1C
N1=C(C=CC=C1)NN.C(C)OC(C(C(C)=O)C=O)=O.N1=CC=CC=C1>>C(C)OC(=O)C=1C(=NN(C1)C1=NC=CC=C1)C
O=[CH:7][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:16](=O)[CH3:17].[NH:8]([c:9]1[cH:10][cH:11][cH:12][cH:13][n:14]1)[NH2:15]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][n:8](-[c:9]2[cH:10][cH:11][cH:12][cH:13][n:14]2)[n:15][c:16]1[CH3:17]
CCOC(=O)C(C=O)C(C)=O.NNc1ccccn1
CCOC(=O)c1cn(-c2ccccn2)nc1C
null
null
C(C)O
Aromatic Heterocycle Formation
Pyrazole formation
d602667e63297ba975a48166d1a7540bdf0e5f502b4608ff23c3d35dbd14c749
78679c7da938d0abe886998033bf74c7e120b260d850498336b36cb336ed2e65
c1ccc(-n2cccn2)nc1
O=[CH;D2;+0:1]-[CH;D3;+0:2](-[C:3](=[O;D1;H0:4])-[#8:5]-[C:6])-[C;H0;D3;+0:7](=O)-[C;D1;H3:8].[NH2;D1;+0:9]-[NH;D2;+0:10]-[c;H0;D3;+0:11](:[#7;a:12]:[c:13]):[c:14]:[c:15]>>[C:6]-[#8:5]-[C:3](=[O;D1;H0:4])-[c;H0;D3;+0:2]1:[cH;D2;+0:1]:[n;H0;D3;+0:10](-[c;H0;D3;+0:11](:[#7;a:12]:[c:13]):[c:14]:[c:15]):[n;H0;D2;+0:9]:[c;H...
null
[]
null
null
null
null
Similar to Example 1, equimolar amounts of 2-pyridylhydrazine and 2-formyl-3-oxo-butyric acid ethyl ester were combined in a solution of 50% pyridine in ethanol. Analysis showed that the resulting solid was determined to be the named product (m.p. 49° C.–50° C.). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Aldehyde.Ketone
Ester
null
c1cn[nH]c1
c1cn[nH]c1.c1ccncc1
HO-
C(C)O
null
null
CCOC(=O)C(C=O)C(C)=O.NNc1ccccn1>C(C)O>CCOC(=O)c1cn(-c2ccccn2)nc1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-96385c6264c1424398d9348e12f7a5f7
CCOC(=O)c1cnn(-c2ccc([N+](=O)[O-])cc2)c1C(F)(F)F>>CCOC(=O)c1cnn(-c2ccc(N)cc2)c1C(F)(F)F
C(=O)[O-].[NH4+].C(C)OC(=O)C=1C=NN(C1C(F)(F)F)C1=CC=C(C=C1)[N+](=O)[O-]>>C(C)OC(=O)C=1C=NN(C1C(F)(F)F)C1=CC=C(C=C1)N
O=[N+:14]([O-])[c:13]1[cH:12][cH:11][c:10](-[n:9]2[n:8][cH:7][c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:17]2[C:18]([F:19])([F:20])[F:21])[cH:16][cH:15]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][n:8][n:9](-[c:10]2[cH:11][cH:12][c:13]([NH2:14])[cH:15][cH:16]2)[c:17]1[C:18]([F:19])([F:20])[F:21]
CCOC(=O)c1cnn(-c2ccc([N+](=O)[O-])cc2)c1C(F)(F)F
CCOC(=O)c1cnn(-c2ccc(N)cc2)c1C(F)(F)F
null
[Pd]
CO
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(-n2cccn2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
8
HOUR
To 1-(4-nitrophenyl)-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (0.5 g, 1.5 mmol) dissolved in methanol (4 mL) was added palladium on carbon and ammonium formate (0.428 g, 6.8 mmol). This mixture was stirred at room temperature overnight. The solvent was removed under vacuum, then the material was resu...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1cn[nH]c1.c1ccccc1
Other
[Pd].CO
null
8
CCOC(=O)c1cnn(-c2ccc([N+](=O)[O-])cc2)c1C(F)(F)F>[Pd].CO>CCOC(=O)c1cnn(-c2ccc(N)cc2)c1C(F)(F)F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8959462339fc4fa39d40a4aaa8d1a18d
O=C(O)C1=CC2C=CC1CC2>>O=C(O)C1=CC2CCC1CC2
C12C(=CC(C=C1)CC2)C(=O)O>>C12C(=CC(CC1)CC2)C(=O)O
[O:1]=[C:2]([OH:3])[C:4]1=[CH:5][CH:6]2[CH:7]=[CH:8][CH:9]1[CH2:10][CH2:11]2>>[O:1]=[C:2]([OH:3])[C:4]1=[CH:5][CH:6]2[CH2:7][CH2:8][CH:9]1[CH2:10][CH2:11]2
O=C(O)C1=CC2C=CC1CC2
O=C(O)C1=CC2CCC1CC2
null
[Pd]
CCOC(=O)C
Reduction
Hydrogenation (double to single)
308380a5c356db5a7568d32bb5139ef654b83c4655b064956b8b4edc3eb3e8f6
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
C1=CC2CCC1CC2
[O;D1;H0:1]=[C:2](-[O;D1;H1:3])-[C:4]1=[C:5]-[C:6]2-[C:7]-[C:8]-[C:9]-1-[CH;D2;+0:10]=[CH;D2;+0:11]-2>>[O;D1;H0:1]=[C:2](-[O;D1;H1:3])-[C:4]1=[C:5]-[C:6]2-[C:7]-[C:8]-[C:9]-1-[CH2;D2;+0:10]-[CH2;D2;+0:11]-2
98.8
[{"value": 98.8, "product": "C12C(=CC(CC1)CC2)C(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
Compound 11A (600 mg, 3.99 mmol) was dissolved in EtOAc (5 mL), 5% Pd/C (12 mg) was added and the mixture was stirred under a hydrogen balloon for 1.5 h. The reaction mixture was filtered through a pad of celite and concentrated under reduced pressure to give 600 mg of compound 11B as a yellow oil. No further purificat...
10.6084/m9.figshare.5104873.v1
null
null
null
C1=CC2C=CC1CC2
C1=CC2CCC1CC2
C1=CC2CCC1CC2
null
[Pd].CCOC(=O)C
null
1.5
O=C(O)C1=CC2C=CC1CC2>[Pd].CCOC(=O)C>O=C(O)C1=CC2CCC1CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1909c0ad6b5f4b5bb7d6bc3e0ee986fa
O=C(Cl)C(=O)Cl.O=C(O)C1=CC2CCC1CC2>>O=C(Cl)C1=CC2CCC1CC2
C(C(=O)Cl)(=O)Cl.C12C(=CC(CC1)CC2)C(=O)O>>C12C(=CC(CC1)CC2)C(=O)Cl
O=C(Cl)C(=O)[Cl:3].O[C:2](=[O:1])[C:4]1=[CH:5][CH:6]2[CH2:7][CH2:8][CH:9]1[CH2:10][CH2:11]2>>[O:1]=[C:2]([Cl:3])[C:4]1=[CH:5][CH:6]2[CH2:7][CH2:8][CH:9]1[CH2:10][CH2:11]2
O=C(Cl)C(=O)Cl.O=C(O)C1=CC2CCC1CC2
O=C(Cl)C1=CC2CCC1CC2
null
CN(C)C=O
C(Cl)Cl
Functional Group Interconversion
Alcohol to chloride_Other
013cec2edeb273a7a148f349d36a52d99ff4e7bcf8eed78085df830088e387ac
aedb1f68dc5b7eb0583043e1125b741382b17974140a2f46554f0110e2ddc884
C1=CC2CCC1CC2
Cl-C(=O)-C(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](=[C:5]-[C:6])-[C:7]>>[C:6]-[C:5]=[C:4](-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3])-[C:7]
100.9
[{"value": 100.9, "product": "C12C(=CC(CC1)CC2)C(=O)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
Oxalyl chloride (2.0 M in CH2Cl2, 2.4 mL, 4.8 mmol, 1.2 eq) was added to a solution of compound 11B (600 mg, 3.95 mmol, 1 eq) in CH2Cl2 (8 mL) containing one drop of DMF. The reaction mixture was stirred at rt for 3 h and then concentrated under reduced pressure to give 680 mg of compound 11C which was used in the next...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Carboxylic acid
Acyl halide
null
null
C1=CC2CCC1CC2
HCl
CN(C)C=O.C(Cl)Cl
null
3
O=C(Cl)C(=O)Cl.O=C(O)C1=CC2CCC1CC2>CN(C)C=O.C(Cl)Cl>O=C(Cl)C1=CC2CCC1CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2975d623528d4c1983bcf37f33b4b1fc
O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C1=CC2CCC1CC2.O=C(OO)c1cccc(Cl)c1>>O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C12OC1C1CCC2CC1
C1=CC(=CC(=C1)Cl)C(=O)OO.[N+](=O)([O-])C1=C(C=C(C=C1)NC(=O)C=1C2CCC(C1)CC2)C(F)(F)F>>[N+](=O)([O-])C1=C(C=C(C=C1)NC(=O)C12C3CCC(C2O1)CC3)C(F)(F)F
[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][c:7]([N+:8](=[O:9])[O-:10])[c:11]([C:12]([F:13])([F:14])[F:15])[cH:16]1)[C:17]1=[CH:19][CH:20]2[CH2:21][CH2:22][CH:23]1[CH2:24][CH2:25]2.O=C(O[OH:18])c1cccc(Cl)c1>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][c:7]([N+:8](=[O:9])[O-:10])[c:11]([C:12]([F:13])([F:14])[F:15])[cH:16]1)[C:17]12[O...
O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C1=CC2CCC1CC2.O=C(OO)c1cccc(Cl)c1
O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C12OC1C1CCC2CC1
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
OtherReaction
f79c34ec388f8df9b9b89ea9de8ecf1ebca4e0f74834a7853952a206f5ce3380
c40ffbbc3249442e5ee39aaa69a55be7ac2fa45f48637395e415c565c1288454
O=C(Nc1ccccc1)C12OC1C1CCC2CC1
Cl-c1:c:c:c:c(-C(=O)-O-[OH;D1;+0:1]):c:1.[O;D1;H0:2]=[C:3](-[#7:4]-[c:5])-[C;H0;D3;+0:6]1=[CH;D2;+0:7]-[C:8]2-[C:9]-[C:10]-[C:11]-1-[C:12]-[C:13]-2>>[O;D1;H0:2]=[C:3](-[#7:4]-[c:5])-[C;H0;D4;+0:6]12-[O;H0;D2;+0:1]-[CH;D3;+0:7]-1-[C:8]1-[C:9]-[C:10]-[C:11]-2-[C:12]-[C:13]-1
58
[{"value": 57.6, "product": "[N+](=O)([O-])C1=C(C=C(C=C1)NC(=O)C12C3CCC(C2O1)CC3)C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 58.0, "product": "[N+](=O)([O-])C1=C(C=C(C=C1)NC(=O)C12C3CCC(C2O1)CC3)C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
mCPBA (60% mixture, 518 mg, 3.00 mmol, 3 eq) was added to a solution of 11D (340 mg, 1.0 mmol, 1.0 eq) in CH2Cl2 (20 mL). The reaction mixture was stirred at rt overnight and then diluted with CH2Cl2 (40 mL). The organic solution was washed with sat. NaHCO3 (1×50 mL), brine (1×50 mL), dried over Na2SO4 and concentrated...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Peroxide
Ether
c1ccccc1.C1=CC2CCC1CC2
C1CC2CCC1C1OC21
c1ccccc1.C1CC2CCC1C1OC21
HCl
C(Cl)Cl
null
8
O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C1=CC2CCC1CC2.O=C(OO)c1cccc(Cl)c1>C(Cl)Cl>O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C12OC1C1CCC2CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-73f63908c360412b9540f8f878a26354
O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C12OC1C1CCC2CC1.O=P(NO)(c1ccccc1)c1ccccc1>>NN(C(=O)C12OC1C1CCC2CC1)c1ccc([N+](=O)[O-])c(C(F)(F)F)c1
[H-].[Na+].[N+](=O)([O-])C1=C(C=C(C=C1)NC(=O)C12C3CCC(C2O1)CC3)C(F)(F)F.C1(=CC=CC=C1)P(=O)(C1=CC=CC=C1)NO>>[N+](=O)([O-])C1=C(C=C(C=C1)N(N)C(=O)C12C3CCC(C2O1)CC3)C(F)(F)F
[NH:2]([C:3](=[O:4])[C:5]12[O:6][CH:7]1[CH:8]1[CH2:9][CH2:10][CH:11]2[CH2:12][CH2:13]1)[c:14]1[cH:15][cH:16][c:17]([N+:18](=[O:19])[O-:20])[c:21]([C:22]([F:23])([F:24])[F:25])[cH:26]1.O=P(c1ccccc1)(c1ccccc1)[NH:1]O>>[NH2:1][N:2]([C:3](=[O:4])[C:5]12[O:6][CH:7]1[CH:8]1[CH2:9][CH2:10][CH:11]2[CH2:12][CH2:13]1)[c:14]1[cH:...
O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C12OC1C1CCC2CC1.O=P(NO)(c1ccccc1)c1ccccc1
NN(C(=O)C12OC1C1CCC2CC1)c1ccc([N+](=O)[O-])c(C(F)(F)F)c1
null
null
CN(C)C=O
Functional Group Addition
OtherReaction
5e05c0c1badc0df2b2150021b18144ee06fc93c19e1707faf0e51ad8dc4ffc92
4b0afe5ae720bad786941c3ee7b748fcbfe464a74354723b418c604097cbd660
O=C(Nc1ccccc1)C12OC1C1CCC2CC1
O-[NH;D2;+0:1]-P(=O)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1.[#8:2]-[C:3]-[C:4](=[O;D1;H0:5])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[#8:2]-[C:3]-[C:4](=[O;D1;H0:5])-[N;H0;D3;+0:6](-[NH2;D1;+0:1])-[c:7](:[c:8]):[c:9]
15.4
[{"value": 15.4, "product": "[N+](=O)([O-])C1=C(C=C(C=C1)N(N)C(=O)C12C3CCC(C2O1)CC3)C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}]
70
CELSIUS
8
HOUR
NaH (60% in mineral oil, 7.9 mg, 0.20 mmol, 1.4 eq) was added to the solution of 11E (50 mg, 0.14 mmol, 1 eq) in DMF (3 mL). The reaction mixture was heated at 70° C. for 2 h. The reaction was cooled to rt and diphenylphosphinylhydroxylamine (52 mg, 0.22 mmol, 1.6 eq, made according to the procedure of Colvin, E. W. et...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Secondary amine
Acylhydrazine
c1ccccc1.c1ccccc1
null
c1ccccc1.C1CC2CCC1C1OC21
HO-
CN(C)C=O
70
8
O=C(Nc1ccc([N+](=O)[O-])c(C(F)(F)F)c1)C12OC1C1CCC2CC1.O=P(NO)(c1ccccc1)c1ccccc1>CN(C)C=O>NN(C(=O)C12OC1C1CCC2CC1)c1ccc([N+](=O)[O-])c(C(F)(F)F)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f742f3db871b4af2af5afa3faa6671a2
COC(=O)C(=O)OC.CSc1ccc(C(C)=O)cc1>>COC(=O)/C(O)=C/C(=O)c1ccc(SC)cc1
COC(C(=O)OC)=O.C[O-].[Na+].Cl.CSC1=CC=C(C=C1)C(C)=O>>O\C(\C(=O)OC)=C/C(=O)C1=CC=C(C=C1)SC
CO[C:5]([C:3]([O:2][CH3:1])=[O:4])=[O:6].[CH3:7][C:8](=[O:9])[c:10]1[cH:11][cH:12][c:13]([S:14][CH3:15])[cH:16][cH:17]1>>[CH3:1][O:2][C:3](=[O:4])/[C:5]([OH:6])=[CH:7]/[C:8](=[O:9])[c:10]1[cH:11][cH:12][c:13]([S:14][CH3:15])[cH:16][cH:17]1
COC(=O)C(=O)OC.CSc1ccc(C(C)=O)cc1
COC(=O)/C(O)=C/C(=O)c1ccc(SC)cc1
null
null
CCOC(=O)C.CCCCCC.C(Cl)Cl.C1(=CC=CC=C1)C
C-C Coupling
OtherReaction
e4a4589a9c43a9e3e18aebd6481c6bd15819939729f59fb85b833b2a820f9d8c
551bf13e9bbf5f86c83696b5ff28a85752492e6b0d2510ee489f6a83816bb6d9
c1ccccc1
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3](=[O;D1;H0:4])-[#8:5]-[C;D1;H3:6].[CH3;D1;+0:7]-[C:8](=[O;D1;H0:9])-[c:10]>>[C;D1;H3:6]-[#8:5]-[C:3](=[O;D1;H0:4])/[C;H0;D3;+0:1](-[OH;D1;+0:2])=[CH;D2;+0:7]/[C:8](=[O;D1;H0:9])-[c:10]
79
[{"value": 79.0, "product": "O\\C(\\C(=O)OC)=C/C(=O)C1=CC=C(C=C1)SC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.9, "product": "O\\C(\\C(=O)OC)=C/C(=O)C1=CC=C(C=C1)SC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
15
MINUTE
Dimethyloxalate (26 g, 180.7 mmol) was added to a stirred suspension of sodium methoxide (9.75 g, 180.7 mmol) in dry toluene (200 mL) at 0° C. The white suspension was stirred for 15 min at 0° C. A solution of 4′-(methylthio)acetophenone (15 g, 90.4 mmol) in dry toluene (150 mL) was then added drop-wise over 15 minutes...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Ester
Ketone.Ester.Enol
null
null
c1ccccc1
HO-
CCOC(=O)C.CCCCCC.C(Cl)Cl.C1(=CC=CC=C1)C
0
0.25
COC(=O)C(=O)OC.CSc1ccc(C(C)=O)cc1>CCOC(=O)C.CCCCCC.C(Cl)Cl.C1(=CC=CC=C1)C>COC(=O)/C(O)=C/C(=O)c1ccc(SC)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d315ddcc6d8d4f5e8190cb9892565d27
CC(=O)c1ccc(C)cc1.COC(=O)C(=O)OC>>COC(=O)C(=O)CC(=O)c1ccc(C)cc1
COC(C(=O)OC)=O.CC1=CC=C(C=C1)C(C)=O>>CC1=CC=C(C=C1)C(CC(C(=O)OC)=O)=O
[CH3:7][C:8](=[O:9])[c:10]1[cH:11][cH:12][c:13]([CH3:14])[cH:15][cH:16]1.CO[C:5]([C:3]([O:2][CH3:1])=[O:4])=[O:6]>>[CH3:1][O:2][C:3](=[O:4])[C:5](=[O:6])[CH2:7][C:8](=[O:9])[c:10]1[cH:11][cH:12][c:13]([CH3:14])[cH:15][cH:16]1
CC(=O)c1ccc(C)cc1.COC(=O)C(=O)OC
COC(=O)C(=O)CC(=O)c1ccc(C)cc1
null
null
null
C-C Coupling
OtherReaction
75e47111412c372865b4b8c2556a24f38f2daf372ab5522938a6e976b4732185
907e247f98c28f5bcc369b20fadcc26c24574c2b68d4b59762f1e8515d373c02
c1ccccc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](=[O;D1;H0:4])-[#8:5]-[C;D1;H3:6].[CH3;D1;+0:7]-[C:8](=[O;D1;H0:9])-[c:10]>>[C;D1;H3:6]-[#8:5]-[C:3](=[O;D1;H0:4])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH2;D2;+0:7]-[C:8](=[O;D1;H0:9])-[c:10]
74
[{"value": 74.0, "product": "CC1=CC=C(C=C1)C(CC(C(=O)OC)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 74.0, "product": "CC1=CC=C(C=C1)C(CC(C(=O)OC)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared from dimethyloxalate (47.24 g, 400 mmol) and 4′-methylacetophenone (26.84 g, 200 mmol) using the procedure for Example 1d. Work-up and recrystallization provided the title compound as white needles (32.6 g, 74% yield). Mp 82–84° C. 1H NMR (300 MHz, CDCl3) δ 15.36 (br.s, 1H), 7.92 (d, J=8...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Ester
Ketone.Ketone
null
null
c1ccccc1
HO-
null
null
null
CC(=O)c1ccc(C)cc1.COC(=O)C(=O)OC>>COC(=O)C(=O)CC(=O)c1ccc(C)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4f84ead693da4f968cd28a52005d8455
NN.NS(=O)(=O)c1ccc(Cl)cc1>>NNc1ccc(S(N)(=O)=O)cc1
ClC1=CC=C(C=C1)S(=O)(=O)N.NN>>N(N)C1=CC=C(C=C1)S(=O)(=O)N
[NH2:1][NH2:2].Cl[c:3]1[cH:4][cH:5][c:6]([S:7]([NH2:8])(=[O:9])=[O:10])[cH:11][cH:12]1>>[NH2:1][NH:2][c:3]1[cH:4][cH:5][c:6]([S:7]([NH2:8])(=[O:9])=[O:10])[cH:11][cH:12]1
NN.NS(=O)(=O)c1ccc(Cl)cc1
NNc1ccc(S(N)(=O)=O)cc1
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
d8df4273e702dfa5f61e1fc063d26292e73a06b19b988689234fbb3a4a4eddc6
61806bbf8bb8981e140ee503663af0ef0e69dc4f34f6582f974a2e4218f7da88
c1ccccc1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[N;D1;H2:6]-[NH2;D1;+0:7]>>[N;D1;H2:6]-[NH;D2;+0:7]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
95
[{"value": 95.0, "product": "N(N)C1=CC=C(C=C1)S(=O)(=O)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 94.8, "product": "N(N)C1=CC=C(C=C1)S(=O)(=O)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A stirred solution of 4-chlorobenzenesulfonamide (38.33 g, 200 mmol) and anhydrous hydrazine (31.4 mL, 1.0 mol) was heated at reflux for 30 hours. After cooling to room temperature, the mixture was poured into water (500 mL) with swirling. The resulting precipitate was collected by filtration, washed thoroughly with wa...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Aromatic halide
Hydrazine
c1ccccc1
c1ccccc1
c1ccccc1
HCl
O
null
null
NN.NS(=O)(=O)c1ccc(Cl)cc1>O>NNc1ccc(S(N)(=O)=O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7a51bd60341c47f6bf110e2467dc0b37
CC(=O)c1cccnc1.COC(=O)C(=O)OC>>COC(=O)C(=O)CC(=O)c1cccnc1
C[O-].[Na+].COC(C(=O)OC)=O.C(C)(=O)C=1C=NC=CC1>>O=C(C(=O)OC)CC(C=1C=NC=CC1)=O
[CH3:7][C:8](=[O:9])[c:10]1[cH:11][cH:12][cH:13][n:14][cH:15]1.CO[C:5]([C:3]([O:2][CH3:1])=[O:4])=[O:6]>>[CH3:1][O:2][C:3](=[O:4])[C:5](=[O:6])[CH2:7][C:8](=[O:9])[c:10]1[cH:11][cH:12][cH:13][n:14][cH:15]1
CC(=O)c1cccnc1.COC(=O)C(=O)OC
COC(=O)C(=O)CC(=O)c1cccnc1
null
null
CO
C-C Coupling
OtherReaction
75e47111412c372865b4b8c2556a24f38f2daf372ab5522938a6e976b4732185
907e247f98c28f5bcc369b20fadcc26c24574c2b68d4b59762f1e8515d373c02
c1ccncc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](=[O;D1;H0:4])-[#8:5]-[C;D1;H3:6].[#7;a:7]:[c:8]:[c:9]-[C:10](-[CH3;D1;+0:11])=[O;D1;H0:12]>>[#7;a:7]:[c:8]:[c:9]-[C:10](=[O;D1;H0:12])-[CH2;D2;+0:11]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](=[O;D1;H0:4])-[#8:5]-[C;D1;H3:6]
84
[{"value": 84.0, "product": "O=C(C(=O)OC)CC(C=1C=NC=CC1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 83.7, "product": "O=C(C(=O)OC)CC(C=1C=NC=CC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
DAY
Sodium methoxide (5.4 g, 100 mmol) and dimethyloxalate (11.8 g, 100 mmol) were dissolved in anhydrous methanol (700 mL) and stirred at room temperature under nitrogen until a suspension was formed. To this mixture, 3-acetylpyridine (5.5 mL, 50 mmol) was added and the stirring was continued for 3 days at room temperatur...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Ester
Ketone.Ketone
null
null
c1ccncc1
HO-
CO
null
72
CC(=O)c1cccnc1.COC(=O)C(=O)OC>CO>COC(=O)C(=O)CC(=O)c1cccnc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-71614f4ee7974ddbb313fb7d2c4b05c4
BrCBr.COC(=O)c1cc(-c2ccc(SC)cc2)n(-c2ccccn2)n1>>CSc1ccc(-c2cc(C(=O)CBr)nn2-c2ccccn2)cc1
CSC1=CC=C(C=C1)C1=CC(=NN1C1=NC=CC=C1)C(=O)OC.BrCBr.C[Li]>>BrCC(=O)C1=NN(C(=C1)C1=CC=C(C=C1)SC)C1=NC=CC=C1
Br[CH2:12][Br:13].CO[C:10]([c:9]1[cH:8][c:7](-[c:6]2[cH:5][cH:4][c:3]([S:2][CH3:1])[cH:23][cH:22]2)[n:15](-[c:16]2[cH:17][cH:18][cH:19][cH:20][n:21]2)[n:14]1)=[O:11]>>[CH3:1][S:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][c:9]([C:10](=[O:11])[CH2:12][Br:13])[n:14][n:15]2-[c:16]2[cH:17][cH:18][cH:19][cH:20][n:21]2)[cH:22][cH...
BrCBr.COC(=O)c1cc(-c2ccc(SC)cc2)n(-c2ccccn2)n1
CSc1ccc(-c2cc(C(=O)CBr)nn2-c2ccccn2)cc1
null
null
C1CCOC1
C-C Coupling
Ester and halide to ketone
ef01edc1b01f560e7b39a38bc55679d327781879123a79598fa9742cc5379d75
50aab8a39d4c72422e6b6f48201993c767ec539687188d0d15e6e0fb0c160b8f
c1ccc(-c2ccnn2-c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[Br;D1;H0:2].C-O-[C;H0;D3;+0:3](=[O;D1;H0:4])-[c:5]1:[#7;a:6]:[#7;a:7](-[c:8]:[#7;a:9]):[c:10]:[c:11]:1>>[#7;a:9]:[c:8]-[#7;a:7]1:[#7;a:6]:[c:5](-[C;H0;D3;+0:3](=[O;D1;H0:4])-[CH2;D2;+0:1]-[Br;D1;H0:2]):[c:11]:[c:10]:1
69
[{"value": 69.0, "product": "BrCC(=O)C1=NN(C(=C1)C1=CC=C(C=C1)SC)C1=NC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 68.7, "product": "BrCC(=O)C1=NN(C(=C1)C1=CC=C(C=C1)SC)C1=NC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
90
MINUTE
To a stirred solution of methyl 5-(4-methylthiophenyl)-1-(2-pyridyl)pyrazole-3-carboxylate (prepared as described in Penning, T. D. et al. J. Med. Chem. 1997, 40, 1347–1365.; 0.39 g, 1.2 mmol) and dibromomethane (0.17 mL, 2.4 mmol) in THF (10 mL) at −78° C. under nitrogen atmosphere was added methyllithium (1.6 M in et...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Ester
Primary halide.Ketone
null
null
c1ccccc1.c1cc[nH]n1.c1ccncc1
HBr
C1CCOC1
null
1.5
BrCBr.COC(=O)c1cc(-c2ccc(SC)cc2)n(-c2ccccn2)n1>C1CCOC1>CSc1ccc(-c2cc(C(=O)CBr)nn2-c2ccccn2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1855fff929db4ad5a02d92ae3b13462a
COC(=O)CCCC(=O)Cl.CSc1ccc(C(C)=O)cc1>>COC(=O)CCCC(=O)/C=C(\O)c1ccc(SC)cc1
ClC(=O)CCCC(=O)OC.O1CCCC1.C(C)(C)[N-]C(C)C.[Li+].C1CCCCC1.CSC1=CC=C(C=C1)C(C)=O.Cl>>O\C(=C/C(CCCC(=O)OC)=O)\C1=CC=C(C=C1)SC
Cl[C:8]([CH2:7][CH2:6][CH2:5][C:3]([O:2][CH3:1])=[O:4])=[O:9].[CH3:10][C:11](=[O:12])[c:13]1[cH:14][cH:15][c:16]([S:17][CH3:18])[cH:19][cH:20]1>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][CH2:6][CH2:7][C:8](=[O:9])/[CH:10]=[C:11](\[OH:12])[c:13]1[cH:14][cH:15][c:16]([S:17][CH3:18])[cH:19][cH:20]1
COC(=O)CCCC(=O)Cl.CSc1ccc(C(C)=O)cc1
COC(=O)CCCC(=O)/C=C(\O)c1ccc(SC)cc1
null
null
C1CCOC1
Acylation
OtherReaction
2029a9fd814fb6888f6b35c6c0956cbe0c2588ea0f802e1fcc4b8a3538ed447f
7af1aa12c8f3746f2a06ac5e1d991bf2e77c1b8a35928ecbdd7fb025269f18f0
c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[CH3;D1;+0:5]-[C;H0;D3;+0:6](=[O;H0;D1;+0:7])-[c:8](:[c:9]):[c:10]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])/[CH;D2;+0:5]=[C;H0;D3;+0:6](\[OH;D1;+0:7])-[c:8](:[c:9]):[c:10]
null
[]
-72
CELSIUS
30
MINUTE
Lithium diisopropylamide mono(tetrahydrofuran) in cyclohexane (1.5 M; 28 mL, 42 mmol) was added to a solution of 1-(4-methylthiophenyl)ethan-1-one (5.16 g, 31 mmol) in THF (120 mL) and stirred for 30 minutes at −72° C. A solution of methyl 4-(chloroformyl)butyrate (1.78 g, 10.8 mmol) was added to the above solution and...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ketone
Ketone.Enol
null
null
c1ccccc1
HCl
C1CCOC1
-72
0.5
COC(=O)CCCC(=O)Cl.CSc1ccc(C(C)=O)cc1>C1CCOC1>COC(=O)CCCC(=O)/C=C(\O)c1ccc(SC)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fd95e3c9024b41f58c60e5039c57717d
NCCCO.O=[N+]([O-])O>>NCCCO[N+](=O)[O-].O=[N+]([O-])O
NCCCO.[N+](=O)(O)[O-]>>[N+](=O)(O)[O-].[N+](=O)([O-])OCCCN
[NH2:1][CH2:2][CH2:3][CH2:4][OH:5].[OH:7][N+:10](=[O:9])[O-:11]>>[NH2:1][CH2:2][CH2:3][CH2:4][O:5][N+:6](=[O:7])[O-:8].[O:9]=[N+:10]([O-:11])[OH:12]
NCCCO.O=[N+]([O-])O
NCCCO[N+](=O)[O-].O=[N+]([O-])O
null
null
C(C)(=O)OC(C)=O
Miscellaneous
OtherReaction
466d5d9cd6feb612ac74d087ae3a5c028119633b42075559ce0b1a6050e470bd
eebe4cdf377c5f23a15ba9981c4bf0f364574de70110a9649086825b36e97a31
null
[C:1]-[C:2]-[OH;D1;+0:3].[O;-;D1;H0:4]-[N+;H0;D3:5](=[O;D1;H0:6])-[OH;D1;+0:7]>>[C:1]-[C:2]-[O;H0;D2;+0:3]-[#7;+:8](-[O;-;D1;H0:9])=[O;H0;D1;+0:7].[O;-;D1;H0:4]-[N+;H0;D3:5](=[O;D1;H0:6])-[O;D1;H1:10]
80
[{"value": 80.0, "product": "[N+](=O)(O)[O-].[N+](=O)([O-])OCCCN", "details": "PERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
A solution of 3-amino-1-propanol (6.17 g, 82.2 mmol) was added, dropwise, to an ice-cooled solution of fuming nitric acid (12 mL) in acetic anhydride (50 mL). The reaction was stirred in an ice-bath for 10 minutes and then at room temperature for 10 minutes. The solvent was evaporated under vacuum at 40° C. The residue...
10.6084/m9.figshare.5104873.v1
null
Nitrate.Primary alcohol
Nitrate.Nitrate
null
null
null
Other
C(C)(=O)OC(C)=O
null
0.166667
NCCCO.O=[N+]([O-])O>C(C)(=O)OC(C)=O>NCCCO[N+](=O)[O-].O=[N+]([O-])O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5c5f16cc6c2d49e0b89c3666d774b67a
CI.COc1cccc2c1C(C)C(=O)N2>>COc1cccc2c1C(C)(C)C(=O)N2
Cl.IC.Cl.C[Si](C)(C)[N-][Si](C)(C)C.[K+].COC1=C2C(C(NC2=CC=C1)=O)C>>COC1=C2C(C(NC2=CC=C1)=O)(C)C
I[CH3:10].[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]2[c:8]1[CH:9]([CH3:11])[C:12](=[O:13])[NH:14]2>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]2[c:8]1[C:9]([CH3:10])([CH3:11])[C:12](=[O:13])[NH:14]2
CI.COc1cccc2c1C(C)C(=O)N2
COc1cccc2c1C(C)(C)C(=O)N2
null
null
CO.O1CCCC1.C1(=CC=CC=C1)C
C-C Coupling
Methylation with MeI_tertiary
4ff962ca13d51fef8dbede7a9389c6828f46295ce155e36b5ca1c7adc5a62f3d
410ec9b1cc243569e4ff568c248f0b402403802e002b4018f576af3f6960507b
O=C1Cc2ccccc2N1
I-[CH3;D1;+0:1].[C;D1;H3:2]-[CH;D3;+0:3]1-[C:4](=[O;D1;H0:5])-[#7:6]-[c:7]:[c:8]-1:[c:9]>>[C;D1;H3:2]-[C;H0;D4;+0:3]1(-[CH3;D1;+0:1])-[C:4](=[O;D1;H0:5])-[#7:6]-[c:7]:[c:8]-1:[c:9]
58
[{"value": 58.0, "product": "COC1=C2C(C(NC2=CC=C1)=O)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 53.1, "product": "COC1=C2C(C(NC2=CC=C1)=O)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
1
HOUR
A solution of 4-methoxy-3-methyl-1,3-dihydro-indol-2-one (41.73 g, 235.5 mmol) and tetrahydrofuran (1000 mL) is cooled to −78° C. Potassium bis(trimethylsilyl)amide (989.0 mL, 494.3 mmol, 0.5 M in toluene) is added over 45 minutes so as to maintain the reaction temperature between −71° C. and −66° C. Iodomethane (36.71...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c(c1)CCN2
c1ccc2c(c1)CCN2
c1ccc2c(c1)CCN2
HI
CO.O1CCCC1.C1(=CC=CC=C1)C
-78
1
CI.COc1cccc2c1C(C)C(=O)N2>CO.O1CCCC1.C1(=CC=CC=C1)C>COc1cccc2c1C(C)(C)C(=O)N2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6e6691a549f845a5a05326a4086fecbe
COc1cccc2c1C(C)(C)C(=O)N2>>CC1(C)C(=O)Nc2cccc(O)c21
Cl.N1=CC=CC=C1.COC1=C2C(C(NC2=CC=C1)=O)(C)C>>OC1=C2C(C(NC2=CC=C1)=O)(C)C
C[O:12][c:11]1[cH:10][cH:9][cH:8][c:7]2[c:13]1[C:2]([CH3:1])([CH3:3])[C:4](=[O:5])[NH:6]2>>[CH3:1][C:2]1([CH3:3])[C:4](=[O:5])[NH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([OH:12])[c:13]21
COc1cccc2c1C(C)(C)C(=O)N2
CC1(C)C(=O)Nc2cccc(O)c21
null
null
CCCCCC
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
O=C1Cc2ccccc2N1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
68.9
[{"value": 68.0, "product": "OC1=C2C(C(NC2=CC=C1)=O)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 68.9, "product": "OC1=C2C(C(NC2=CC=C1)=O)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
220
CELSIUS
45
MINUTE
Pyridine hydrochloride (51.10 g, 442.2 mmol) and 4-methoxy-3,3-dimethyl-1,3-dihydro-indol-2-one (21.61 g, 113.0 mmol) are combined and stirred in a melt at 220° C. for 45 minutes. Heating is removed and when the mixture cooled to 100° C., water (60 mL) is added, followed by ethyl acetate (150 mL) at 65° C. The layers a...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccc2c(c1)CCN2
Other
CCCCCC
220
0.75
COc1cccc2c1C(C)(C)C(=O)N2>CCCCCC>CC1(C)C(=O)Nc2cccc(O)c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e4c5726ac3974685a58e1ea2a6c0c8f7
CC(C)[N+](=O)[O-].CN(C)Cc1c[nH]c2c(OCc3ccccc3)cccc12>>CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]
[N+](=O)([O-])C(C)C.CN(C)CC1=CNC2=C1C=CC=C2OCC3=CC=CC=C3.[OH-].[Na+].[N+](=O)([O-])C(C)C>>CC(CC1=CNC2=C(C=CC=C12)OCC1=CC=CC=C1)(C)[N+](=O)[O-]
[CH3:1][CH:2]([CH3:3])[N+:22](=[O:23])[O-:24].CN(C)[CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([O:10][CH2:11][c:12]3[cH:13][cH:14][cH:15][cH:16][cH:17]3)[cH:18][cH:19][cH:20][c:21]12>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([O:10][CH2:11][c:12]3[cH:13][cH:14][cH:15][cH:16][cH:17]3)[cH:18][cH:19][cH:20][c:21...
CC(C)[N+](=O)[O-].CN(C)Cc1c[nH]c2c(OCc3ccccc3)cccc12
CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]
null
null
CCOCC
C-C Coupling
OtherReaction
410d0ecf550dfec32b5bd37f61aeafc75533d5e4329aa3110c08acb15e21dcaa
fc73a0ba4f6f90cb21df47612bcde105fcd2a049cd56b52924f944fc6a6cbe55
c1ccc(COc2cccc3cc[nH]c23)cc1
C-N(-C)-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:1.[C;D1;H3:7]-[CH;D3;+0:8](-[C;D1;H3:9])-[#7;+:10](-[O;-;D1;H0:11])=[O;D1;H0:12]>>[C;D1;H3:7]-[C;H0;D4;+0:8](-[C;D1;H3:9])(-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:1)-[#7;+:10](-[O;-;D1;H0:11])=[O;D1;H0:12]
92.1
[{"value": 92.0, "product": "CC(CC1=CNC2=C(C=CC=C12)OCC1=CC=CC=C1)(C)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.1, "product": "CC(CC1=CNC2=C(C=CC=C12)OCC1=CC=CC=C1)(C)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
29
HOUR
A mixture of 7-benzyloxy gramine (1.99 g, 7.10 mmol), solid NaOH (298 mg, 7.22 mmol) and 2-nitropropane (4.5 mL, 50 mmol) is heated to reflux. After 10 minutes at reflux, a thick slurry developed which is difficult to stir. Gas evolution is observed, and an additional 1 mL of 2-nitropropane is added to loosen the mixtu...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Tertiary amine
Nitro group
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
Other
CCOCC
null
29
CC(C)[N+](=O)[O-].CN(C)Cc1c[nH]c2c(OCc3ccccc3)cccc12>CCOCC>CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b83aba9157f44fd9b0f7974734e9190c
CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]>>CC(C)(N)Cc1c[nH]c2c(OCc3ccccc3)cccc12
CC(CC1=CNC2=C(C=CC=C12)OCC1=CC=CC=C1)(C)[N+](=O)[O-].C(C)O>>CC(CC1=CNC2=C(C=CC=C12)OCC1=CC=CC=C1)(C)N
O=[N+:4]([O-])[C:2]([CH3:1])([CH3:3])[CH2:5][c:6]1[cH:7][nH:8][c:9]2[c:10]([O:11][CH2:12][c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)[cH:19][cH:20][cH:21][c:22]12>>[CH3:1][C:2]([CH3:3])([NH2:4])[CH2:5][c:6]1[cH:7][nH:8][c:9]2[c:10]([O:11][CH2:12][c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)[cH:19][cH:20][cH:21][c:22]12
CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]
CC(C)(N)Cc1c[nH]c2c(OCc3ccccc3)cccc12
null
[Ni]
O1CCCC1
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(COc2cccc3cc[nH]c23)cc1
O=[N+;H0;D3:1](-[O-])-[C:2](-[C:3])(-[C;D1;H3:4])-[C;D1;H3:5]>>[C:3]-[C:2](-[C;D1;H3:4])(-[C;D1;H3:5])-[NH2;D1;+0:1]
99
[{"value": 99.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
60
CELSIUS
1
HOUR
A mixture of 3-(2-methyl-2-nitropropyl)-7-(benzyloxy)indole (25.0 g, 77.1 mmol), Raney Nickel® (9.5 g wet lump), and 3A ethanol (250 mL) is pressurized to 50 psig with H2 and is heated to 60° C. After 1 hour, the mixture is cooled to ambient temperature. The mixture is diluted with tetrahydrofuran (100 mL) and is warme...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
Other
[Ni].O1CCCC1
60
1
CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]>[Ni].O1CCCC1>CC(C)(N)Cc1c[nH]c2c(OCc3ccccc3)cccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9dc9d58956fe4180abe509a7f0f59e1e
CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC1=CC=CC=C1)(C)C)=O>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)O)(C)C)=O
c1ccc(C[O:10][c:9]2[c:8]3[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:15][C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])[c:14]3[cH:13][cH:12][cH:11]2)cc1>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([OH:10])[cH:11][cH:12][cH:13][c:14]12)[NH:15][C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21...
CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)NC(=O)OC(C)(C)C
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C
null
[Pd]
C(C)O
Deprotection
Hydroxyl benzyl deprotection
36869d1fe85185a14d9eb30bf05178c600a9b6eca277ffaf3803578c30e0bf5d
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1ccc2[nH]ccc2c1
[c:1]:[c:2](-[O;H0;D2;+0:3]-C-c1:c:c:c:c:c:1):[c:4](:[c:5]):[#7;a:6]:[c:7]>>[OH;D1;+0:3]-[c:2](:[c:1]):[c:4](:[c:5]):[#7;a:6]:[c:7]
96.2
[{"value": 96.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)O)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.2, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)O)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
40
MINUTE
A mixture of [2-(7-benzyloxy-1H-indol-3-yl)-1,1-dimethyl-ethyl]-carbamic acid tert-butyl ester (20.75 g, 52.6 mmol), 5% Pd/C (1.00 g, 5 wt %), and 3A ethanol (200 mL) is pressurized to 55 psig with H2, and is heated to 50° C. After 40 minutes, the slurry is filtered, and the filtrate is concentrated to give 15.41 g of ...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
c1ccccc1
null
c1ccc2[nH]ccc2c1
Other
[Pd].C(C)O
50
0.666667
CC(C)(Cc1c[nH]c2c(OCc3ccccc3)cccc12)NC(=O)OC(C)(C)C>[Pd].C(C)O>CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-32cf1dfce18849a1889085ab34daa5ed
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.NC(=O)c1ccc(Br)cc1>>CC(C)(Cc1c[nH]c2c(-c3ccc(C(N)=O)cc3)cccc12)NC(=O)OC(C)(C)C
BrC1=CC=C(C(=O)N)C=C1.B1(OC(C(O1)(C)C)(C)C)B2OC(C(O2)(C)C)(C)C.C(C)(=O)[O-].[K+].C(C)(C)(C)OC(=O)NC(CC1=CNC2=C(C=CC=C12)OS(=O)(=O)C(F)(F)F)(C)C.C([O-])([O-])=O.[Na+].[Na+]>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CC=C(C=C1)C(N)=O)(C)C)=O
O=S(=O)(O[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:23][C:24](=[O:25])[O:26][C:27]([CH3:28])([CH3:29])[CH3:30])[c:22]2[cH:21][cH:20][cH:19]1)C(F)(F)F.Br[c:10]1[cH:11][cH:12][c:13]([C:14]([NH2:15])=[O:16])[cH:17][cH:18]1>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9](-[c:10]3[cH:11][cH:...
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.NC(=O)c1ccc(Br)cc1
CC(C)(Cc1c[nH]c2c(-c3ccc(C(N)=O)cc3)cccc12)NC(=O)OC(C)(C)C
null
null
C(C)(=O)OCC.CS(=O)C.[Cl-].[Na+].O
C-C Coupling
OtherReaction
1b2df86b67777cac54c7612bb407c72c2c13320e3c623fa8dcc9aa27a39bb9ba
6fa0c5f5a567aef7a3c8790e894c3eacfb3f5a56b34ccd5ba5e56676973c2603
c1ccc(-c2cccc3cc[nH]c23)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]):[c:4]:[c:5]
58.5
[{"value": 58.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CC=C(C=C1)C(N)=O)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 58.5, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CC=C(C=C1)C(N)=O)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
20
CELSIUS
null
null
A solution of 4-bromobenzamide (150 mg, 0.75 mmol), bis(pinacolato)diboron (209 mg, 0.825 mmol), potassium acetate (0.221 g, 2.25 mmol) and {1,1′-bis(diphenylphosphino)-ferrocene}dichloropalladium dichloromethane complex (18 mg, 0.0225 mmol) in dimethylsulfoxide (5 mL) is heated to 80° C. for two hours. The mixture is ...
10.6084/m9.figshare.5104873.v1
null
Triflate.Aromatic halide
null
c1ccc2[nH]ccc2c1.c1ccccc1
c1ccccc1.c1ccc2[nH]ccc2c1
c1ccccc1.c1ccc2[nH]ccc2c1
TfOH.Br-
C(C)(=O)OCC.CS(=O)C.[Cl-].[Na+].O
20
null
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.NC(=O)c1ccc(Br)cc1>C(C)(=O)OCC.CS(=O)C.[Cl-].[Na+].O>CC(C)(Cc1c[nH]c2c(-c3ccc(C(N)=O)cc3)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1bf2a222fc824b4c96663fff97db984b
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccc(C(F)(F)F)cc1>>CC(C)(Cc1c[nH]c2c(-c3ccc(C(F)(F)F)cc3)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(=O)NC(CC1=CNC2=C(C=CC=C12)OS(=O)(=O)C(F)(F)F)(C)C.C([O-])([O-])=O.[Na+].[Na+].FC(C1=CC=C(C=C1)B(O)O)(F)F>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CC=C(C=C1)C(F)(F)F)(C)C)=O
O=S(=O)(O[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31])[c:23]2[cH:22][cH:21][cH:20]1)C(F)(F)F.OB(O)[c:10]1[cH:11][cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][cH:19]1>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9](-[c:10]3[cH...
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccc(C(F)(F)F)cc1
CC(C)(Cc1c[nH]c2c(-c3ccc(C(F)(F)F)cc3)cccc12)NC(=O)OC(C)(C)C
null
[Pd].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.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
O1CCCC1.[Cl-].[Na+].O
C-C Coupling
Suzuki coupling with boronic acids OTf
e5b06a5a12e240e2c1d187f11833a1f8be82588ba5052d6ae155510c885c9487
3f602cf53fbcf2a56d992979503f6bea55727095a6b9075475a711784170b440
c1ccc(-c2cccc3cc[nH]c23)cc1
F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].O-B(-O)-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]>>[c:10]:[c:9]:[c;H0;D3;+0:8](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]):[c:11]:[c:12]
93.3
[{"value": 93.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CC=C(C=C1)C(F)(F)F)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.3, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CC=C(C=C1)C(F)(F)F)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of trifluoro-methanesulfonic acid 3-(2-tert-butoxycarbonylamino-2-methyl-propyl)-1H-indol-7-yl ester (305 mg, 0.699 mmol) in tetrahydrofuran (4.5 mL) is added sodium carbonate (1 mL, 2M, 2 mmol), tetrakis(triphenylphosphine)-palladium (32 mg, 0.0280 mmol) and 4-trifluoromethylbenzeneboronic acid (0.1 99 g...
10.6084/m9.figshare.5104873.v1
null
Triflate.Boronic acid
null
c1ccc2[nH]ccc2c1.c1ccccc1
c1ccccc1.c1ccc2[nH]ccc2c1
c1ccccc1.c1ccc2[nH]ccc2c1
TfOH.HO-.B
[Pd].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.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.O1CCCC1.[Cl-].[Na+].O
null
null
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccc(C(F)(F)F)cc1>[Pd].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.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.O1CCCC1.[Cl-].[Na+].O>CC(C)(Cc1c[nH]c2c(-c3ccc(C(F)(F)F)cc3)cccc12)NC(=O)OC...
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-61c1e1a0aa5e442d91a796b5a4f41109
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccsc1>>CC(C)(Cc1c[nH]c2c(-c3ccsc3)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(=O)NC(CC1=CNC2=C(C=CC=C12)OS(=O)(=O)C(F)(F)F)(C)C.C(C)N(CC)CC.S1C=C(C=C1)B(O)O>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CSC=C1)(C)C)=O
O=S(=O)(O[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:19][C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[c:18]2[cH:17][cH:16][cH:15]1)C(F)(F)F.OB(O)[c:10]1[cH:11][cH:12][s:13][cH:14]1>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9](-[c:10]3[cH:11][cH:12][s:13][cH:14]3)[cH:15][cH:...
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccsc1
CC(C)(Cc1c[nH]c2c(-c3ccsc3)cccc12)NC(=O)OC(C)(C)C
null
[Pd].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.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
C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O
C-C Coupling
Suzuki coupling with boronic acids OTf
a7850579aaea4f63726c5ab350ab1102424a87584a5eae5768d335f9a6e0784b
3f602cf53fbcf2a56d992979503f6bea55727095a6b9075475a711784170b440
c1cc(-c2ccsc2)c2[nH]ccc2c1
F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].O-B(-O)-[c;H0;D3;+0:8]1:[c:9]:[c:10]:[#16;a:11]:[c:12]:1>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:8]1:[c:9]:[c:10]:[#16;a:11]:[c:12]:1):[c:4](:[c:5]):[#7;a:6]:[c:7]
69
[{"value": 69.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CSC=C1)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 68.6, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=CSC=C1)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of trifluoro-methanesulfonic acid 3-(2-tert-butoxycarbonylamino-2-methyl-propyl)-1H-indol-7-yl ester (340 mg, 0.779 mmol) in dimethylformamide (5 mL) is added triethylamine (0.14 mL, 1.01 mmol), tetrakis(triphenylphosphine)-palladium (36 mg, 0.0312 mmol) and 3-thiopheneboronic acid (130 mg, 1.01 mmol). Th...
10.6084/m9.figshare.5104873.v1
null
Triflate.Boronic acid
null
c1ccc2[nH]ccc2c1.c1ccsc1
c1ccsc1.c1ccc2[nH]ccc2c1
c1ccsc1.c1ccc2[nH]ccc2c1
TfOH.HO-.B
[Pd].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.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.C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O
null
null
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccsc1>[Pd].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.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.C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O>CC(C)(Cc1c[nH]c2c(-c3ccsc3)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0732badd337946498b912644452a820b
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1cccs1>>CC(C)(Cc1c[nH]c2c(-c3cccs3)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(=O)NC(CC1=CNC2=C(C=CC=C12)OS(=O)(=O)C(F)(F)F)(C)C.C(C)N(CC)CC.S1C(=CC=C1)B(O)O>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C=1SC=CC1)(C)C)=O
O=S(=O)(O[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:19][C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[c:18]2[cH:17][cH:16][cH:15]1)C(F)(F)F.OB(O)[c:10]1[cH:11][cH:12][cH:13][s:14]1>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9](-[c:10]3[cH:11][cH:12][cH:13][s:14]3)[cH:15][cH:...
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1cccs1
CC(C)(Cc1c[nH]c2c(-c3cccs3)cccc12)NC(=O)OC(C)(C)C
null
[Pd].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.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
C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O
C-C Coupling
Suzuki coupling with boronic acids OTf
a7850579aaea4f63726c5ab350ab1102424a87584a5eae5768d335f9a6e0784b
3f602cf53fbcf2a56d992979503f6bea55727095a6b9075475a711784170b440
c1csc(-c2cccc3cc[nH]c23)c1
F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].O-B(-O)-[c;H0;D3;+0:8]1:[#16;a:9]:[c:10]:[c:11]:[c:12]:1>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:8]1:[#16;a:9]:[c:10]:[c:11]:[c:12]:1):[c:4](:[c:5]):[#7;a:6]:[c:7]
31.3
[{"value": 31.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C=1SC=CC1)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 31.3, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C=1SC=CC1)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of trifluoro-methanesulfonic acid 3-(2-tert-butoxycarbonylamino-2-methyl-propyl)-1H-indol-7-yl ester (437 mg, 1.00 mmol) in dimethylformamide (6 mL) is added triethylamine (0.18 mL, 1.30 mmol), tetrakis(triphenylphosphine)-palladium (46 mg, 0.0401 mmol) and 2-thiopheneboronic acid (167 mg, 1.30 mmol). The...
10.6084/m9.figshare.5104873.v1
null
Triflate.Boronic acid
null
c1ccc2[nH]ccc2c1.c1ccsc1
c1ccsc1.c1ccc2[nH]ccc2c1
c1ccsc1.c1ccc2[nH]ccc2c1
TfOH.HO-.B
[Pd].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.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.C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O
null
null
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1cccs1>[Pd].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.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.C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O>CC(C)(Cc1c[nH]c2c(-c3cccs3)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-343aac3f52b94d84a607d6578897d0f3
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccc(C(F)(F)F)cc1C(F)(F)F>>CC(C)(Cc1c[nH]c2c(-c3ccc(C(F)(F)F)cc3C(F)(F)F)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(=O)NC(CC1=CNC2=C(C=CC=C12)OS(=O)(=O)C(F)(F)F)(C)C.C(C)N(CC)CC.FC(C1=C(C=CC(=C1)C(F)(F)F)B(O)O)(F)F>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=C(C=C(C=C1)C(F)(F)F)C(F)(F)F)(C)C)=O
O=S(=O)(O[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:28][C:29](=[O:30])[O:31][C:32]([CH3:33])([CH3:34])[CH3:35])[c:27]2[cH:26][cH:25][cH:24]1)C(F)(F)F.OB(O)[c:10]1[cH:11][cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][c:19]1[C:20]([F:21])([F:22])[F:23]>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][n...
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccc(C(F)(F)F)cc1C(F)(F)F
CC(C)(Cc1c[nH]c2c(-c3ccc(C(F)(F)F)cc3C(F)(F)F)cccc12)NC(=O)OC(C)(C)C
null
[Pd].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.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
C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O
C-C Coupling
Suzuki coupling with boronic acids OTf
e5b06a5a12e240e2c1d187f11833a1f8be82588ba5052d6ae155510c885c9487
3f602cf53fbcf2a56d992979503f6bea55727095a6b9075475a711784170b440
c1ccc(-c2cccc3cc[nH]c23)cc1
F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].O-B(-O)-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11](-[C:12](-[F;D1;H0:13])(-[F;D1;H0:14])-[F;D1;H0:15]):[c:16]>>[F;D1;H0:13]-[C:12](-[F;D1;H0:14])(-[F;D1;H0:15])-[c:11](:[c:16]):[c;H0;D3;+0:8](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]...
89.2
[{"value": 89.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=C(C=C(C=C1)C(F)(F)F)C(F)(F)F)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.2, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C1=C(C=C(C=C1)C(F)(F)F)C(F)(F)F)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
To a solution of trifluoro-methanesulfonic acid 3-(2-tert-butoxycarbonylamino-2-methyl-propyl)-1H-indol-7-yl ester (262 mg, 0.600 mmol) in dimethylformamide (3.5 mL) is added triethylamine (0.11 mL, 0.780 mmol), tetrakis(triphenylphosphine)-palladium (28 mg, 0.0240 mmol) and 2,4-bistrifluoromethylbenzeneboronic acid (2...
10.6084/m9.figshare.5104873.v1
null
Triflate.Boronic acid
null
c1ccc2[nH]ccc2c1.c1ccccc1
c1ccccc1.c1ccc2[nH]ccc2c1
c1ccccc1.c1ccc2[nH]ccc2c1
TfOH.HO-.B
[Pd].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.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.C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O
100
null
CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C.OB(O)c1ccc(C(F)(F)F)cc1C(F)(F)F>[Pd].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.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.C(C)(=O)OCC.CN(C=O)C.[Cl-].[Na+].O>CC(C)(Cc1c[nH]c2c(-c3ccc(C(F)(F)...
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-30b6def8a1514691b9d38b1893394da3
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.N#CCBr>>CC(C)(Cc1c[nH]c2c(OCC#N)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)O)(C)C)=O.BrCC#N.C(=O)([O-])[O-].[K+].[K+]>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC#N)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([OH:10])[cH:14][cH:15][cH:16][c:17]12)[NH:18][C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25].Br[CH2:11][C:12]#[N:13]>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([O:10][CH2:11][C:12]#[N:13])[cH:14][cH:15][cH:16][c:17]12)[NH:18][C:19](=[O:...
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.N#CCBr
CC(C)(Cc1c[nH]c2c(OCC#N)cccc12)NC(=O)OC(C)(C)C
null
null
CC(CC)=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccc2[nH]ccc2c1
Br-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7](:[c:8]):[#7;a:9]:[c:10]>>[N;D1;H0:3]#[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7](:[c:8]):[#7;a:9]:[c:10]
86.5
[{"value": 86.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC#N)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.5, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC#N)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A mixture of [2-(7-hydroxy-1H-indol-3-yl)-1,1-dimethyl-ethyl]-carbamic acid tert-butyl ester (15.55 g, 51.1 mmol), bromoacetonitrile (10.7 mL, 153 mmol), K2CO3 (17.78 g, 128.6 mmol) and 2-butanone is heated to reflux. After 1 hour the mixture is allowed to cool and is filtered through celite. The filtrate is concentrat...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccc2[nH]ccc2c1
HBr
CC(CC)=O
null
1
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.N#CCBr>CC(CC)=O>CC(C)(Cc1c[nH]c2c(OCC#N)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d323c67d08ed4629b72f93d0bf5352fc
CC(=Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]>>CC(N)Cc1c[nH]c2c(OCc3ccccc3)cccc12
[H-].[Al+3].[Li+].[H-].[H-].[H-].C(C1=CC=CC=C1)OC=1C=CC=C2C(=CNC12)C=C(C)[N+](=O)[O-].[H-].[Al+3].[Li+].[H-].[H-].[H-]>>C(C1=CC=CC=C1)OC=1C=CC=C2C(=CNC12)CC(C)N
O=[N+:3]([O-])[C:2]([CH3:1])=[CH:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([O:10][CH2:11][c:12]3[cH:13][cH:14][cH:15][cH:16][cH:17]3)[cH:18][cH:19][cH:20][c:21]12>>[CH3:1][CH:2]([NH2:3])[CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([O:10][CH2:11][c:12]3[cH:13][cH:14][cH:15][cH:16][cH:17]3)[cH:18][cH:19][cH:20][c:21]12
CC(=Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]
CC(N)Cc1c[nH]c2c(OCc3ccccc3)cccc12
null
null
O1CCCC1
Reduction
OtherReaction
4337e4e8b75c4193a30be38c3139251eb50201a1e90dac1ecfc293dd3e226a46
1ad3bfd18d4cba7c52a6c2c4705cfa4e2dc99589d9555154a809489f21a7a436
c1ccc(COc2cccc3cc[nH]c23)cc1
O=[N+;H0;D3:1](-[O-])-[C;H0;D3;+0:2](-[C;D1;H3:3])=[CH;D2;+0:4]-[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:1>>[C;D1;H3:3]-[CH;D3;+0:2](-[NH2;D1;+0:1])-[CH2;D2;+0:4]-[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:1
null
[]
30
CELSIUS
2
HOUR
Lithium aluminum hydride (LAH, 24 g, 600 mmol) is added portionwise to dry tetrahydrofuran (1800 mL) at −5° C. to 5° C. A solution of the nitroolefin from above (61.6 g, 200 mmol) in tetrahydrofuran (1200 mL) is added to the LAH solution over 30 minutes while maintaining the temperature at −5° C. to 5° C. When the addi...
10.6084/m9.figshare.5104873.v1
null
Enamine
Primary amine
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
Other
O1CCCC1
30
2
CC(=Cc1c[nH]c2c(OCc3ccccc3)cccc12)[N+](=O)[O-]>O1CCCC1>CC(N)Cc1c[nH]c2c(OCc3ccccc3)cccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-579ccc08061142699e0875fb06cf892e
CC(Cc1c[nH]c2c(OCc3ccccc3)cccc12)NC(=O)OC(C)(C)C.N#CCBr>>CC(Cc1c[nH]c2c(OCC#N)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC1=CC=CC=C1)C)=O.BrCC#N.C([O-])([O-])=O.[K+].[K+]>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC#N)C)=O
c1ccc(C[O:9][c:8]2[c:7]3[nH:6][cH:5][c:4]([CH2:3][CH:2]([CH3:1])[NH:17][C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[c:16]3[cH:15][cH:14][cH:13]2)cc1.Br[CH2:10][C:11]#[N:12]>>[CH3:1][CH:2]([CH2:3][c:4]1[cH:5][nH:6][c:7]2[c:8]([O:9][CH2:10][C:11]#[N:12])[cH:13][cH:14][cH:15][c:16]12)[NH:17][C:18](=[O:19])[O:2...
CC(Cc1c[nH]c2c(OCc3ccccc3)cccc12)NC(=O)OC(C)(C)C.N#CCBr
CC(Cc1c[nH]c2c(OCC#N)cccc12)NC(=O)OC(C)(C)C
null
null
C(C)C(=O)C
Heteroatom Alkylation and Arylation
OtherReaction
e33314bc856efe080a739af2d51cb97bb8af73b526448347bb35795fea2551a7
969a4609e178674696657c590a647839ca01abd1f90b8f0c9e475b1d6507651b
c1ccc2[nH]ccc2c1
Br-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3].[c:4]:[c:5](-[O;H0;D2;+0:6]-C-c1:c:c:c:c:c:1):[c:7](:[c:8]):[#7;a:9]:[c:10]>>[N;D1;H0:3]#[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[c:5](:[c:4]):[c:7](:[c:8]):[#7;a:9]:[c:10]
70.2
[{"value": 70.2, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC#N)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
The crude {1-methyl-2-[7-hydroxy-1H-indol-3-yl]ethyl}-carbamic acid tert-butyl ester from above (29.2 g, 102 mmol theory) is dissolved in methyl ethyl ketone (300 mL) and bromoacetonitrile (20.4 mL, 306 mmol) and potassium carbonate (33.8 g, 250 mmol) is added. The mixture is heated at 80° C. for 2 hours. The solids ar...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether
Ether
c1ccccc1
null
c1ccc2[nH]ccc2c1
HBr
C(C)C(=O)C
80
null
CC(Cc1c[nH]c2c(OCc3ccccc3)cccc12)NC(=O)OC(C)(C)C.N#CCBr>C(C)C(=O)C>CC(Cc1c[nH]c2c(OCC#N)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c661d089a084439e8ed863fc8eb54792
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.N#Cc1cccnc1Cl>>CC(C)(Cc1c[nH]c2c(Oc3ncccc3C#N)cccc12)NC(=O)OC(C)(C)C
O.ClC1=C(C#N)C=CC=N1.C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)O)(C)C)=O.[H-].[Na+]>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OC1=NC=CC=C1C#N)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([OH:10])[cH:19][cH:20][cH:21][c:22]12)[NH:23][C:24](=[O:25])[O:26][C:27]([CH3:28])([CH3:29])[CH3:30].Cl[c:11]1[n:12][cH:13][cH:14][cH:15][c:16]1[C:17]#[N:18]>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([O:10][c:11]3[n:12][cH:13][cH:14][cH:15][c:...
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.N#Cc1cccnc1Cl
CC(C)(Cc1c[nH]c2c(Oc3ncccc3C#N)cccc12)NC(=O)OC(C)(C)C
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
99925b30dd2603ae575cba81b58435d015cd6b7267cf347380904f25833af5f2
27e9a6bab4e3ed54aeb6be4d84cb1c0170208288795e252a46e57e44ecc064f0
c1ccc(Oc2cccc3cc[nH]c23)nc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[OH;D1;+0:8]-[c:9](:[c:10]):[c:11](:[c:12]):[#7;a:13]:[c:14]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[O;H0;D2;+0:8]-[c:9](:[c:10]):[c:11](:[c:12]):[#7;a:13]:[c:14]):[#7;a:2]:[c:3]
96
[{"value": 96.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OC1=NC=CC=C1C#N)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.7, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OC1=NC=CC=C1C#N)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
25
MINUTE
To a solution of [2-(7-Hydroxy-1H-indol-3-yl)-1,1-dimethyl-ethyl]-carbamic acid tert-butyl ester (274 mg, 0.900 mmol) in dimethylformamide (15 mL) is added sodium hydride (26 mg, 1.07 mmol). The mixture is stirred at ambient temperature for 25 minutes under nitrogen. 2-Chloro-nicotinonitrile (187 mg, 1.35 mmol) is adde...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic alcohol
Ether
c1ccncc1
c1ccncc1
c1ccncc1.c1ccc2[nH]ccc2c1
HCl
CN(C=O)C
null
0.416667
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.N#Cc1cccnc1Cl>CN(C=O)C>CC(C)(Cc1c[nH]c2c(Oc3ncccc3C#N)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-738a85bc0da5412e8b8a396e20525741
CC(C)(Cc1c[nH]c2c(Oc3ncccc3C#N)cccc12)NC(=O)OC(C)(C)C>>CCCCCCCCCCCCN
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OC1=NC=CC=C1C#N)(C)C)=O.O1CCOCC1.Cl.O1CCOCC1>>CCCCCCCCCCCCN
C[C:2](OC(=O)[NH:13][C:12](C[c:5]1c[nH]c2c(Oc3ncccc3C#N)ccc[c:6]21)([CH3:1])[CH3:11])([CH3:3])[CH3:4]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][NH2:13]
CC(C)(Cc1c[nH]c2c(Oc3ncccc3C#N)cccc12)NC(=O)OC(C)(C)C
CCCCCCCCCCCCN
null
null
null
Miscellaneous
OtherReaction
388918355f7c8f9bb89414f7093a44d1c359462eea2423ba0f1998be4941eede
f44468835921508c0283ab83a9324a4767b46169709243988fd96217b6f79842
null
C-[C;H0;D4;+0:1](-[CH3;D1;+0:2])(-[CH3;D1;+0:3])-O-C(=O)-[NH;D2;+0:4]-[C;H0;D4;+0:5](-[CH3;D1;+0:6])(-[CH3;D1;+0:7])-C-[c;H0;D3;+0:8]1:c:[nH]:c2:[c;H0;D3;+0:9]:1:c:c:c:c:2-O-c1:n:c:c:c:c:1-C#N>>[CH3;D1;+0:7]-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[CH2;D2;+0:3]-[CH2;D2;+0:8]-[CH2;D2;+0:9]-[C:10]-[C:11]-[C:12]-[C:13]-[CH2;D2;+0:6]-...
83
[{"value": 83.0, "product": "CCCCCCCCCCCCN", "details": "PERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
{2-[7-(3-Cyano-pyridin-2-yloxy)-1H-indol-3-yl]-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester (119 mg, 0.293 mmol) is dissolved in 10 mL of 1,4 dioxane. The mixture is cooled to zero degrees Celsius in an ice/water bath. To the mixture is added 10 mL of 4N hydrochloric acid in 1,4 dioxane, and the resulting mixture...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Nitrile.Boc
Primary amine
c1ccncc1.c1ccc2[nH]ccc2c1
null
null
Other
null
null
5
CC(C)(Cc1c[nH]c2c(Oc3ncccc3C#N)cccc12)NC(=O)OC(C)(C)C>>CCCCCCCCCCCCN
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cf0e1cb12fbf4ee49772ed33ad4ad6b7
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.COC(=O)c1ccc(Cl)nc1>>COC(=O)c1ccc(Oc2cccc3c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c23)nc1
O.COC(C1=CN=C(C=C1)Cl)=O.C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)O)(C)C)=O.[H-].[Na+]>>COC(C1=CN=C(C=C1)OC=1C=CC=C2C(=CNC12)CC(C)(C)NC(=O)OC(C)(C)C)=O
[OH:9][c:10]1[cH:11][cH:12][cH:13][c:14]2[c:15]([CH2:16][C:17]([CH3:18])([CH3:19])[NH:20][C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27])[cH:28][nH:29][c:30]12.Cl[c:8]1[cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:32][n:31]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([O:9][c:10]2[cH:11][cH:12][cH:13][c...
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.COC(=O)c1ccc(Cl)nc1
COC(=O)c1ccc(Oc2cccc3c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c23)nc1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
99925b30dd2603ae575cba81b58435d015cd6b7267cf347380904f25833af5f2
27e9a6bab4e3ed54aeb6be4d84cb1c0170208288795e252a46e57e44ecc064f0
c1ccc(Oc2cccc3cc[nH]c23)nc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5].[OH;D1;+0:6]-[c:7](:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]>>[c:8]:[c:7](-[O;H0;D2;+0:6]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5]):[c:9](:[c:10]):[#7;a:11]:[c:12]
58
[{"value": 58.0, "product": "COC(C1=CN=C(C=C1)OC=1C=CC=C2C(=CNC12)CC(C)(C)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 57.9, "product": "COC(C1=CN=C(C=C1)OC=1C=CC=C2C(=CNC12)CC(C)(C)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of [2-(7-hydroxy-1H-indol-3-yl)-1,1-dimethyl-ethyl]-carbamic acid tert-butyl ester (104 mg, 0.342 mmol) in dimethylformamide (10 mL) is added sodium hydride (10 mg, 0.410 mmol). The mixture is stirred at ambient temperature for 30 minutes under nitrogen. 6-Chloro-nicotinic acid methyl ester (99 mg, 0.581 ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic alcohol
Ether
c1ccncc1
c1ccncc1
c1ccncc1.c1ccc2[nH]ccc2c1
HCl
CN(C=O)C
null
0.5
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.COC(=O)c1ccc(Cl)nc1>CN(C=O)C>COC(=O)c1ccc(Oc2cccc3c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c23)nc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-891086c3a8cc43c7beb58f68c0a282e1
Cc1csc2ccccc12.O=C1CCC(=O)N1Br>>BrCc1csc2ccccc12
CC=1C2=C(SC1)C=CC=C2.C1CC(=O)N(C1=O)Br.N(=NC(C#N)(C)C)C(C#N)(C)C>>BrCC=1C2=C(SC1)C=CC=C2
[CH3:2][c:3]1[cH:4][s:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]12.O=C1CCC(=O)N1[Br:1]>>[Br:1][CH2:2][c:3]1[cH:4][s:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]12
Cc1csc2ccccc12.O=C1CCC(=O)N1Br
BrCc1csc2ccccc12
null
null
C(Cl)(Cl)(Cl)Cl
Functional Group Interconversion
Wohl-Ziegler bromination benzyl primary
45c0aca0d63a96f0092e6dded9c888827eaf6379dac179e1cefc99293896300a
08f5e7e34d3f321cce3e85421b38226d6240cca0939494ae61032d4f8405cf22
c1ccc2sccc2c1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3]1:[c:4]:[c:5]:[#16;a:6]:[c:7]:1>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3]1:[c:4]:[c:5]:[#16;a:6]:[c:7]:1
42.2
[{"value": 42.0, "product": "BrCC=1C2=C(SC1)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 42.2, "product": "BrCC=1C2=C(SC1)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
3-Methylbenzo[b]thiophene (9.9 g, 67 mmol) is heated in carbon tetrachloride (133 ml ) to near reflux in the presence of n-bromosuccinimide (11.9 g, 67 mmol, 1.0 eq.). 2,2′Azobisisobutyronitrile (2.2 g, 13.3 mmol, 0.2 eq.) is added and the resulting mixture is refluxed for two hours. After cooling, the reaction mixture...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Primary halide
C1CCNC1
null
c1ccc2sccc2c1
HO-
C(Cl)(Cl)(Cl)Cl
null
null
Cc1csc2ccccc12.O=C1CCC(=O)N1Br>C(Cl)(Cl)(Cl)Cl>BrCc1csc2ccccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f19b2da9cf8f4cdb9a4858498d10bf19
C[C@H]1CO1.c1ccc2c(c1)CCN2>>CC(O)CN1CCc2ccccc21
N1CCC2=CC=CC=C12.C1[C@H](C)O1>>OC(CN1CCC2=CC=CC=C12)C
[CH3:1][C@@H:2]1[O:3][CH2:4]1.[NH:5]1[CH2:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]21>>[CH3:1][CH:2]([OH:3])[CH2:4][N:5]1[CH2:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]21
C[C@H]1CO1.c1ccc2c(c1)CCN2
CC(O)CN1CCc2ccccc21
null
null
C(C)O
Heteroatom Alkylation and Arylation
Ring opening of epoxide with amine
d4379babff0daffbed1781da20aedf50f4924ca02a809782fe33166d88fdc20d
97e758d6c4c8255d25541eb6c6a6f62e7dc30829ea162ca3392731efabc98a65
c1ccc2c(c1)CCN2
[C;D1;H3:1]-[C@H;D3;+0:2]1-[CH2;D2;+0:3]-[O;H0;D2;+0:4]-1.[c:5]:[c:6]1:[c:7]-[C:8]-[C:9]-[NH;D2;+0:10]-1>>[C;D1;H3:1]-[CH;D3;+0:2](-[OH;D1;+0:4])-[CH2;D2;+0:3]-[N;H0;D3;+0:10]1-[C:9]-[C:8]-[c:7]:[c:6]-1:[c:5]
63
[{"value": 63.0, "product": "OC(CN1CCC2=CC=CC=C12)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.9, "product": "OC(CN1CCC2=CC=CC=C12)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 2,3-dihydro-1H-indole (5.74 g, 48.2 mmol), and (S)-propylene oxide (2.8 g, 48.2 mmol) in ethanol (200 mL) is heated at reflux for 18 hours. The resulting mixture is cooled to room temperature, and evaporated to give a crude oil. The material is purified by flash chromatography (25% ethyl acetate/hexanes) t...
10.6084/m9.figshare.5104873.v1
null
Ether.Secondary amine
Secondary alcohol.Tertiary amine
C1CO1.c1ccc2c(c1)CCN2
c1ccc2c(c1)CC[NH]2
c1ccc2c(c1)CC[NH]2
null
C(C)O
null
null
C[C@H]1CO1.c1ccc2c(c1)CCN2>C(C)O>CC(O)CN1CCc2ccccc21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6f7c251455c743cbaee5673ee07fb180
CC(C)(Cc1c[nH]c2c(OCC(=O)O)cccc12)NC(=O)OC(C)(C)C.CN>>CNC(=O)COc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
C(C)(C)(C)OC(=O)NC(CC1=CNC2=C(C=CC=C12)OCC(=O)O)(C)C.CN>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC(NC)=O)(C)C)=O
O[C:3](=[O:4])[CH2:5][O:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([CH2:13][C:14]([CH3:15])([CH3:16])[NH:17][C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[cH:25][nH:26][c:27]12.[CH3:1][NH2:2]>>[CH3:1][NH:2][C:3](=[O:4])[CH2:5][O:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([CH2:13][C:14]([CH3:15])([CH3:16])[NH:17][...
CC(C)(Cc1c[nH]c2c(OCC(=O)O)cccc12)NC(=O)OC(C)(C)C.CN
CNC(=O)COc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
null
null
CN(C=O)C
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
c1ccc2[nH]ccc2c1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#8:4].[C;D1;H3:5]-[NH2;D1;+0:6]>>[#8:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:6]-[C;D1;H3:5]
100.9
[{"value": 75.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC(NC)=O)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 100.9, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)OCC(NC)=O)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a solution of [2-(7-cyanomethoxy-1H-indol-3-yl)-1,1-dimethyl-ethyl]-carbamic acid tert-butyl ester (3.8 mmol) is added 2 N NaOH (10.0 mL, 20 mmol). The reaction mixture is reluxed for 2 hours. The reaction mixture is cooled to room temperature, evaporated to about 10 mL, acidified to pH 3.0 with 1 N HCl. The mixture...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccc2[nH]ccc2c1
HO-
CN(C=O)C
null
3
CC(C)(Cc1c[nH]c2c(OCC(=O)O)cccc12)NC(=O)OC(C)(C)C.CN>CN(C=O)C>CNC(=O)COc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d71cbd8395f942d6899bd3f39091693f
C=CC(=O)OC.CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>COC(=O)C=Cc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
C(C)(C)(C)OC(=O)NC(CC1=CNC2=C(C=CC=C12)OS(=O)(=O)C(F)(F)F)(C)C.C(C=C)(=O)OC.C(C)N(CC)CC.C(C)(=O)OCC>>COC(C=CC=1C=CC=C2C(=CNC12)CC(C)(C)NC(=O)OC(C)(C)C)=O
[CH3:1][O:2][C:3](=[O:4])[CH:5]=[CH2:6].O=S(=O)(O[c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([CH2:13][C:14]([CH3:15])([CH3:16])[NH:17][C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[cH:25][nH:26][c:27]12)C(F)(F)F>>[CH3:1][O:2][C:3](=[O:4])[CH:5]=[CH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([CH2:13][C:14]([CH3:15])(...
C=CC(=O)OC.CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C
COC(=O)C=Cc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
null
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
CN(C=O)C.[Cl-].[Na+].O
C-C Coupling
OtherReaction
f6e4dd56ea32f13c678e29217fd0c4333a51cf64229efe954763e2e76edb3e0c
e84d2ff35b106b73e905407d80ffdd5c53fba81bdf3725d58511290daa9d3d79
c1ccc2[nH]ccc2c1
F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].[C;D1;H3:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[C:12]=[CH2;D1;+0:13]>>[C;D1;H3:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[C:12]=[CH;D2;+0:13]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]
82
[{"value": 82.0, "product": "COC(C=CC=1C=CC=C2C(=CNC12)CC(C)(C)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 81.7, "product": "COC(C=CC=1C=CC=C2C(=CNC12)CC(C)(C)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
90
CELSIUS
8
HOUR
Trifluoro-methanesulfonic acid 3-(2-tert-butoxycarbonylamino-2-methyl-propyl)-1H-indol-7-yl ester (200 mg, 0.46 mmol), methyl acrylate (80 mg, 0.92 mmol) and triethylamine (0.40 mL, 3.0 mmol) is stirred in dimethylformamide (2.0 mL) at room temperature for 30 minutes. Dichlorobis(triphenylphosphine)palladium (31 mg, 0....
10.6084/m9.figshare.5104873.v1
null
Triflate.Vinyl
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
TfOH.HO-
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.CN(C=O)C.[Cl-].[Na+].O
90
8
C=CC(=O)OC.CC(C)(Cc1c[nH]c2c(OS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.CN(C=O)C.[Cl-].[Na+].O>COC(=O)C=Cc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e3ca42b23ffb4a7196121ed97b6f0eec
COC(=O)C=Cc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12>>COC(=O)CCc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CCS(=O)(=O)C)(C)C)=O.COC(C=CC=1C=CC=C2C(=CNC12)CC(C)(C)NC(=O)OC(C)(C)C)=O>>COC(CCC=1C=CC=C2C(=CNC12)CC(C)(C)NC(=O)OC(C)(C)C)=O
[CH3:1][O:2][C:3](=[O:4])[CH:5]=[CH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([CH2:13][C:14]([CH3:15])([CH3:16])[NH:17][C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[cH:25][nH:26][c:27]12>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][CH2:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([CH2:13][C:14]([CH3:15])([CH3:16])[NH:17][C:...
COC(=O)C=Cc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
COC(=O)CCc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
null
null
null
Reduction
Hydrogenation (double to single)
c04c38f95d7b746e5bdb99c368a7a33956c97b95b54c7ad89be2a85526386ec9
9a50abf8d2e4cd9195d7a0cadbe97483a261a81cf70b653cfddd5ecf76d383a6
c1ccc2[nH]ccc2c1
[C;D1;H3:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH;D2;+0:5]=[CH;D2;+0:6]-[c:7](:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]>>[C;D1;H3:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[c:7](:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]
null
[]
null
null
null
null
3-[3-(2-tert-Butoxycarbonylamino-2-methyl-propyl)-1H-indol-7-yl]-propionic acid methyl ester is prepared from 3-[3-(2-tert-butoxycarbonylamino-2-methyl-propyl)-1H-indol-7-yl]-acrylic acid methyl ester as described below for the preparation of {2-[7-(2-methanesulfonyl-ethyl)-1H-indol-3-yl]-1,1-dimethyl-ethyl}-carbamic a...
10.6084/m9.figshare.5104873.v1
null
Ester
Ester
null
null
c1ccc2[nH]ccc2c1
null
null
null
null
COC(=O)C=Cc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12>>COC(=O)CCc1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-95f19424f7b140e69f40dc1b673ed663
C=CC(N)=O.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=CC(N)=O)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CS(=O)(=O)C(F)(F)F)(C)C)=O.C(C=C)(=O)N>>C(C)(C)(C)OC(=O)NC(CC1=CNC2=C(C=CC=C12)C=CC(=O)N)(C)C
[CH2:10]=[CH:11][C:12]([NH2:13])=[O:14].O=S(=O)(C[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:19][C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[c:18]2[cH:17][cH:16][cH:15]1)C(F)(F)F>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([CH:10]=[CH:11][C:12]([NH2:13])=[O:14])[cH:15][cH...
C=CC(N)=O.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C
CC(C)(Cc1c[nH]c2c(C=CC(N)=O)cccc12)NC(=O)OC(C)(C)C
null
null
null
C-C Coupling
OtherReaction
9ee5c848b3529c0571d068ce5ea5cd4d1d3705da2182d3214d2c9187dbcdd8d9
9a367fc6597a2c2d2ef687b5d530f141dc98e4ffcb30f47f73afa833e2c55025
c1ccc2[nH]ccc2c1
F-C(-F)(-F)-S(=O)(=O)-C-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].[CH2;D1;+0:8]=[C:9]-[C:10](-[N;D1;H2:11])=[O;D1;H0:12]>>[N;D1;H2:11]-[C:10](=[O;D1;H0:12])-[C:9]=[CH;D2;+0:8]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]
null
[]
null
null
null
null
3-[3-(2-tert-Butoxycarbonylamino-2-methyl-propyl)-1H-indol-7-yl]-acrylamide is prepared from [1,1-dimethyl-2-(7-trifluoromethanesulfonylmethyl-1H-indol-3-yl)-ethyl]-carbamic acid tert-butyl ester and acrylamide as described for the preparation of Amine 23 (98%). FDMS m/e 356.2 (M++1). Conditions: See reaction.notes.pro...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Sulfone.Vinyl
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
HF
null
null
null
C=CC(N)=O.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=CC(N)=O)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6bb9173e2bfb4e009592dee1e206c9e3
C=CS(C)(=O)=O.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=CS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CS(=O)(=O)C(F)(F)F)(C)C)=O.C(=C)S(=O)(=O)C>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C=CS(=O)(=O)C)(C)C)=O
[CH2:10]=[CH:11][S:12]([CH3:13])(=[O:14])=[O:15].O=S(=O)(C[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:20][C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27])[c:19]2[cH:18][cH:17][cH:16]1)C(F)(F)F>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([CH:10]=[CH:11][S:12]([CH3:13])(=[O:14])...
C=CS(C)(=O)=O.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C
CC(C)(Cc1c[nH]c2c(C=CS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
null
null
null
C-C Coupling
OtherReaction
9ee5c848b3529c0571d068ce5ea5cd4d1d3705da2182d3214d2c9187dbcdd8d9
9a367fc6597a2c2d2ef687b5d530f141dc98e4ffcb30f47f73afa833e2c55025
c1ccc2[nH]ccc2c1
F-C(-F)(-F)-S(=O)(=O)-C-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].[#16:8]-[C:9]=[CH2;D1;+0:10]>>[#16:8]-[C:9]=[CH;D2;+0:10]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]
null
[]
null
null
null
null
{2-[7-(2-Methanesulfonyl-vinyl)-1H-indol-3-yl)-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester is prepared from [1,1-dimethyl-2-(7-trifluoromethanesulfonylmethyl-1H-indol-3-yl)-ethyl]-carbamic acid tert-butyl ester and methyl vinyl sulfone as described for the preparation of Amine 23 (98%). FDMS m/e=392.2 (M++1). Co...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Sulfone.Vinyl
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
HF
null
null
null
C=CS(C)(=O)=O.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=CS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2b811ded5cc54bc39f20d5cd39b68575
CC(C)(Cc1c[nH]c2c(C=CS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(CCS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C=CS(=O)(=O)C)(C)C)=O>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CCS(=O)(=O)C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([CH:10]=[CH:11][S:12]([CH3:13])(=[O:14])=[O:15])[cH:16][cH:17][cH:18][c:19]12)[NH:20][C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27]>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([CH2:10][CH2:11][S:12]([CH3:13])(=[O:14])=[O:15])[cH:16][cH:...
CC(C)(Cc1c[nH]c2c(C=CS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
CC(C)(Cc1c[nH]c2c(CCS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
null
[Pd]
CO
Reduction
Hydrogenation (double to single)
0bc3968b35f0839c230afb4215314da278abd4e1f10e42ec3012c5512de49ea5
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1ccc2[nH]ccc2c1
[C;D1;H3:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[CH;D2;+0:5]=[CH;D2;+0:6]-[c:7](:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]>>[C;D1;H3:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[c:7](:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]
80
[{"value": 80.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CCS(=O)(=O)C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.6, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CCS(=O)(=O)C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of {2-[7-(2-methanesulfonyl-vinyl)-1H-indol-3-yl]-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester (0.40 g, 1.02,mmol) in methanol (20.0 mL) is added 10% Pd/C (0.10 g) in methanol (2.0 mL). The reaction mixture is purged with hydrogen and hydrogenation is carried out with a hydrogen balloon overnight. T...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccc2[nH]ccc2c1
null
[Pd].CO
null
null
CC(C)(Cc1c[nH]c2c(C=CS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C>[Pd].CO>CC(C)(Cc1c[nH]c2c(CCS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cc06287670bb4fbd823adbb3133bb5b9
C=CC#N.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=CC#N)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CS(=O)(=O)C(F)(F)F)(C)C)=O.C(C=C)#N>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C=CC#N)(C)C)=O
[CH2:10]=[CH:11][C:12]#[N:13].O=S(=O)(C[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:18][C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])[c:17]2[cH:16][cH:15][cH:14]1)C(F)(F)F>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([CH:10]=[CH:11][C:12]#[N:13])[cH:14][cH:15][cH:16][c:17]12)...
C=CC#N.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C
CC(C)(Cc1c[nH]c2c(C=CC#N)cccc12)NC(=O)OC(C)(C)C
null
null
null
C-C Coupling
OtherReaction
9ee5c848b3529c0571d068ce5ea5cd4d1d3705da2182d3214d2c9187dbcdd8d9
9a367fc6597a2c2d2ef687b5d530f141dc98e4ffcb30f47f73afa833e2c55025
c1ccc2[nH]ccc2c1
F-C(-F)(-F)-S(=O)(=O)-C-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].[CH2;D1;+0:8]=[C:9]-[C:10]#[N;D1;H0:11]>>[N;D1;H0:11]#[C:10]-[C:9]=[CH;D2;+0:8]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]
null
[]
null
null
null
null
{2-[7-(2-Cyano-vinyl)-1H-indol-3-yl]-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester is prepared from [1,1-dimethyl-2-(7-trifluoromethanesulfonylmethyl-1H-indol-3-yl)-ethyl]-carbamic acid tert-butyl ester and acrylonitrile as described for the preparation of Amine 23 (85%). FDMS m/e=339.2 (M++1). Conditions: See rea...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Sulfone.Vinyl
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
HF
null
null
null
C=CC#N.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=CC#N)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-71909e61d7c54e33a7c5b60a56e3b72e
CCOC(=O)Cl.Nc1c(F)cc(F)cc1Br>>CCOC(=O)Nc1c(F)cc(F)cc1Br
C(C)(=O)OCC.CCCCCC.BrC1=C(N)C(=CC(=C1)F)F.ClC(=O)OCC>>BrC1=C(NC(=O)OCC)C(=CC(=C1)F)F
Cl[C:4]([O:3][CH2:2][CH3:1])=[O:5].[NH2:6][c:7]1[c:8]([F:9])[cH:10][c:11]([F:12])[cH:13][c:14]1[Br:15]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH:6][c:7]1[c:8]([F:9])[cH:10][c:11]([F:12])[cH:13][c:14]1[Br:15]
CCOC(=O)Cl.Nc1c(F)cc(F)cc1Br
CCOC(=O)Nc1c(F)cc(F)cc1Br
null
null
N1=CC=CC=C1
Protection
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
038720aa61a7efa0f2a9ee6f2e0adf63a9ffdc2be4697c11a6215baef34f97b2
205f353513ce9506ab61831799da8fb73ec2ef5cfa927664496d3ce72c438860
c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[C:4]-[#8:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]
94
[{"value": 94.0, "product": "BrC1=C(NC(=O)OCC)C(=CC(=C1)F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.7, "product": "BrC1=C(NC(=O)OCC)C(=CC(=C1)F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a vigorously stirred solution of 2-bromo-4,6-difluoro aniline (100 g, 0.48 mol) in pyridine (400 mL), at 0° C., is added ethyl chloroformate (70 ml, 0.73 mol) at a rate to keep the temperature below 5° C. When addition is complete, the mixture is stirred at 0° C.–5° C. an additional 2 hours while monitoring by TLC (...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether.Primary amine
Carbamic ester
null
null
c1ccccc1
HCl
N1=CC=CC=C1
null
null
CCOC(=O)Cl.Nc1c(F)cc(F)cc1Br>N1=CC=CC=C1>CCOC(=O)Nc1c(F)cc(F)cc1Br
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-05f580e2ae4c4a0682b6fb32ae9bb51f
C#C[Si](C)(C)C.CCOC(=O)Nc1c(F)cc(F)cc1Br>>CCOC(=O)Nc1c(F)cc(F)cc1C#C[Si](C)(C)C
BrC1=C(NC(=O)OCC)C(=CC(=C1)F)F.C(C)N(CC)CC.C[Si](C)(C)C#C>>C[Si](C)(C)C#CC1=C(NC(=O)OCC)C(=CC(=C1)F)F
[CH:15]#[C:16][Si:17]([CH3:18])([CH3:19])[CH3:20].Br[c:14]1[c:7]([NH:6][C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:8]([F:9])[cH:10][c:11]([F:12])[cH:13]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH:6][c:7]1[c:8]([F:9])[cH:10][c:11]([F:12])[cH:13][c:14]1[C:15]#[C:16][Si:17]([CH3:18])([CH3:19])[CH3:20]
C#C[Si](C)(C)C.CCOC(=O)Nc1c(F)cc(F)cc1Br
CCOC(=O)Nc1c(F)cc(F)cc1C#C[Si](C)(C)C
null
[Cu]I.Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
CC#N
C-C Coupling
Sonogashira alkyne_aryl halide
15c08902746c61a960c314898ce6bb5fcc5e189f9e057388c59dba9ec9d0c81c
305eca0fd2975da49e7f69e4edfb9dc1cbce82513954bc5a73be3289e70e5f76
c1ccccc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7:5]-[C:6]=[O;D1;H0:7]):[c:8].[C;D1;H3:9]-[#14:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C:13]#[CH;D1;+0:14]>>[C;D1;H3:9]-[#14:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C:13]#[C;H0;D2;+0:14]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7:5]-[C:6]=[O;D1;H0:7]):[c:8]
71
[{"value": 71.0, "product": "C[Si](C)(C)C#CC1=C(NC(=O)OCC)C(=CC(=C1)F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 67.3, "product": "C[Si](C)(C)C#CC1=C(NC(=O)OCC)C(=CC(=C1)F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
In a 2 L flask, 2-bromo-4,6-difluoro-N-carbethoxy aniline (42 g, 150 mmol) in CH3CN (500 mL) is degassed with vacuum and purged with N2. Dichlorobis(triphenylphosphine)palladium(II) (10.5 g, 15 mmol, 10 mol %), followed by CuI (710 mg, 4 mmol, 2.5 mol %) and triethyl amine (41 mL) are added and rinsed in with 100 mL of...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Alkyne
Alkyne
c1ccccc1
c1ccccc1
c1ccccc1
HBr
[Cu]I.Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.CC#N
null
null
C#C[Si](C)(C)C.CCOC(=O)Nc1c(F)cc(F)cc1Br>[Cu]I.Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.CC#N>CCOC(=O)Nc1c(F)cc(F)cc1C#C[Si](C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a9d09bb02bf34689b618636a056c80b1
CCOC(=O)Nc1c(F)cc(F)cc1C#C[Si](C)(C)C>>CC[O-].Fc1cc(F)c2[nH]ccc2c1
[H-].[Na+].C[Si](C)(C)C#CC1=C(NC(=O)OCC)C(=CC(=C1)F)F.C(C)(=O)OCC.CCCCCC>>[O-]CC.[Na+].FC=1C=C2C=CNC2=C(C1)F
C[Si](C)(C)C#[C:12][c:13]1[c:9]([NH:10][C:11](=O)[O:3][CH2:2][CH3:1])[c:7]([F:8])[cH:6][c:5]([F:4])[cH:14]1>>[CH3:1][CH2:2][O-:3].[F:4][c:5]1[cH:6][c:7]([F:8])[c:9]2[nH:10][cH:11][cH:12][c:13]2[cH:14]1
CCOC(=O)Nc1c(F)cc(F)cc1C#C[Si](C)(C)C
CC[O-].Fc1cc(F)c2[nH]ccc2c1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
d93159aaafb07623ac70398631606f6fda7f6909e2825456e8155a5393ab3f67
96f6078eb7a094b71a64f7dd2ec28cce2fb0038aa097ceee40707bfd91d8a122
c1ccc2[nH]ccc2c1
C-[Si](-C)(-C)-C#[C;H0;D2;+0:1]-[c:2](:[c:3]):[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:6](=O)-[O;H0;D2;+0:7]-[C:8]-[C;D1;H3:9]):[c:10]>>[C;D1;H3:9]-[C:8]-[O-;H0;D1:7].[c:3]:[c:2]1:[cH;D2;+0:1]:[cH;D2;+0:6]:[nH;D2;+0:5]:[c:4]:1:[c:10]
78.4
[{"value": 78.0, "product": "FC=1C=C2C=CNC2=C(C1)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.4, "product": "FC=1C=C2C=CNC2=C(C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Fresh sodium ethoxide is prepared by carefully adding NaH (16 g of 60% oil dispersion, 400 mmol) to 550 mL of ethanol under N2. 2-(Trimethylsilylethynyl)-4,6-difluoro-N-carbethoxyaniline (28 g, 100 mmol) in 150 mL of ethanol is added and reaction is stirred at room temperature approximately 45 minutes, while monitoring...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Alkyne.Silyl protective group
null
c1ccccc1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
HO-
C(C)O
null
null
CCOC(=O)Nc1c(F)cc(F)cc1C#C[Si](C)(C)C>C(C)O>CC[O-].Fc1cc(F)c2[nH]ccc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-563d6e04fa2144da9e95cdda593c8abd
ClI.Fc1cc(F)c2[nH]ccc2c1.O=S(=O)(Cl)c1ccccc1>>O=S(=O)(c1ccccc1)n1cc(I)c2cc(F)cc(F)c21
C1(=CC=CC=C1)S(=O)(=O)Cl.ICl.C(Cl)Cl.FC=1C=C2C=CNC2=C(C1)F>>C1(=CC=CC=C1)S(=O)(=O)N1C=C(C2=CC(=CC(=C12)F)F)I
Cl[I:13].[nH:10]1[cH:11][cH:12][c:14]2[cH:15][c:16]([F:17])[cH:18][c:19]([F:20])[c:21]12.Cl[S:2](=[O:1])(=[O:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][cH:9]1>>[O:1]=[S:2](=[O:3])([c:4]1[cH:5][cH:6][cH:7][cH:8][cH:9]1)[n:10]1[cH:11][c:12]([I:13])[c:14]2[cH:15][c:16]([F:17])[cH:18][c:19]([F:20])[c:21]12
ClI.Fc1cc(F)c2[nH]ccc2c1.O=S(=O)(Cl)c1ccccc1
O=S(=O)(c1ccccc1)n1cc(I)c2cc(F)cc(F)c21
null
[Br-].C(CCC)[N+](CCCC)(CCCC)CCCC
N1=CC=CC=C1.[OH-].[Na+].C1(=CC=CC=C1)C
Miscellaneous
OtherReaction
65c4847c06bac21126f9fb144209ef63ce8313245b1b724a321d6cd031cec566
51ac21fb371666dad6c719abf761fc77677c24795c2c33a15b0a4d5159f01965
O=S(=O)(c1ccccc1)n1ccc2ccccc21
Cl-[I;H0;D1;+0:1].Cl-[S;H0;D4;+0:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c:5](:[c:6]):[c:7].[c:8]:[c:9]1:[cH;D2;+0:10]:[c:11]:[nH;D2;+0:12]:[c:13]:1:[c:14]>>[I;H0;D1;+0:1]-[c;H0;D3;+0:10]1:[c:11]:[n;H0;D3;+0:12](-[S;H0;D4;+0:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c:5](:[c:6]):[c:7]):[c:13](:[c:14]):[c:9]:1:[c:8]
87
[{"value": 87.0, "product": "C1(=CC=CC=C1)S(=O)(=O)N1C=C(C2=CC(=CC(=C12)F)F)I", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
The 1.0 M ICl in CH2Cl2 (43 ml, 43 mmol) is added to a solution of 5,7-difluoroindole (6 g, 39 mmol) in 35 ml pyridine under N2 at 0° C. and the resulting mixture is stirred for 30 minutes. The reaction is diluted with toluene and washed with brine, 1N HCl, 1N NaOH, dried (Na2SO4), filtered and concentrated. The crude ...
10.6084/m9.figshare.5104873.v1
null
Sulfonyl halide
Aromatic halide
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccccc1.c1ccc2[nH]ccc2c1
HCl
[Br-].C(CCC)[N+](CCCC)(CCCC)CCCC.N1=CC=CC=C1.[OH-].[Na+].C1(=CC=CC=C1)C
null
0.5
ClI.Fc1cc(F)c2[nH]ccc2c1.O=S(=O)(Cl)c1ccccc1>[Br-].C(CCC)[N+](CCCC)(CCCC)CCCC.N1=CC=CC=C1.[OH-].[Na+].C1(=CC=CC=C1)C>O=S(=O)(c1ccccc1)n1cc(I)c2cc(F)cc(F)c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-399e2e2cad6e47cab2717298fec2cb59
CC(C(O)c1cn(S(=O)(=O)c2ccccc2)c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1>>C[C@@H](Cc1c[nH]c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1
[H-].[Al+3].[Li+].[H-].[H-].[H-].C(C1=CC=CC=C1)N(CC1=CC=CC=C1)C(C(O)C1=CN(C2=C(C=C(C=C12)F)F)S(=O)(=O)C1=CC=CC=C1)C>>C(C1=CC=CC=C1)N([C@H](CC1=CNC2=C(C=C(C=C12)F)F)C)CC1=CC=CC=C1
O=S(=O)(c1ccccc1)[n:6]1[cH:5][c:4]([CH:3](O)[CH:2]([CH3:1])[N:15]([CH2:16][c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[CH2:23][c:24]2[cH:25][cH:26][cH:27][cH:28][cH:29]2)[c:14]2[c:7]1[c:8]([F:9])[cH:10][c:11]([F:12])[cH:13]2>>[CH3:1][C@@H:2]([CH2:3][c:4]1[cH:5][nH:6][c:7]2[c:8]([F:9])[cH:10][c:11]([F:12])[cH:13][c:14]1...
CC(C(O)c1cn(S(=O)(=O)c2ccccc2)c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1
C[C@@H](Cc1c[nH]c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1
null
null
O1CCOCC1.O1CCCC1
Reduction
OtherReaction
314558446aae30b1e0db2c7845b84a181628981e07c25fc4a354bd6222968a70
46f8a11b80b06e754a5a34198d843342612a5e7ede950bda52ce3a500cedba0b
c1ccc(CN(CCc2c[nH]c3ccccc23)Cc2ccccc2)cc1
O-[CH;D3;+0:1](-[CH;D3;+0:2](-[C;D1;H3:3])-[#7:4](-[C:5])-[C:6])-[c:7]1:[c:8]:[c:9](:[c:10]):[n;H0;D3;+0:11](-S(=O)(=O)-c2:c:c:c:c:c:2):[c:12]:1>>[C:5]-[#7:4](-[C:6])-[C@@H;D3;+0:2](-[C;D1;H3:3])-[CH2;D2;+0:1]-[c:7]1:[c:8]:[c:9](:[c:10]):[nH;D2;+0:11]:[c:12]:1
93.1
[{"value": 86.0, "product": "C(C1=CC=CC=C1)N([C@H](CC1=CNC2=C(C=C(C=C12)F)F)C)CC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.1, "product": "C(C1=CC=CC=C1)N([C@H](CC1=CNC2=C(C=C(C=C12)F)F)C)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Lithium aluminum hydride (LAH) (0.7 g, 18 mmol) is added portionwise to a dioxane/tetrahydrofuran (90 ml/10 ml) solution of 2-(N,N-dibenzylamino)-1-(1-benzenesulfonyl-5,7-difluoro-1H-indol-3-yl)-propan-1-ol (1.9 g, 3.3 mmol) under N2 at 0° C. After the addition is complete, the reaction is allowed to warm to room tempe...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
null
c1ccccc1.c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1.c1ccccc1
HO-
O1CCOCC1.O1CCCC1
null
null
CC(C(O)c1cn(S(=O)(=O)c2ccccc2)c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1>O1CCOCC1.O1CCCC1>C[C@@H](Cc1c[nH]c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-825e0f147af6474489eb0897d71af069
CI.C[C@H](Cc1c[nH]c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1>>C[C@H](Cc1cn(C)c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1
[H-].[Na+].C(C1=CC=CC=C1)N([C@@H](CC1=CNC2=C(C=C(C=C12)F)F)C)CC1=CC=CC=C1.IC>>C(C1=CC=CC=C1)N([C@@H](CC1=CN(C2=C(C=C(C=C12)F)F)C)C)CC1=CC=CC=C1
I[CH3:7].[CH3:1][C@H:2]([CH2:3][c:4]1[cH:5][nH:6][c:8]2[c:9]([F:10])[cH:11][c:12]([F:13])[cH:14][c:15]12)[N:16]([CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1)[CH2:24][c:25]1[cH:26][cH:27][cH:28][cH:29][cH:30]1>>[CH3:1][C@H:2]([CH2:3][c:4]1[cH:5][n:6]([CH3:7])[c:8]2[c:9]([F:10])[cH:11][c:12]([F:13])[cH:14][c:15]12...
CI.C[C@H](Cc1c[nH]c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1
C[C@H](Cc1cn(C)c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
5f4295751cbf2eac77c77b599ebb727e1800dd106de3a7476670f0ac76dbeba5
7a358c636daddc97c1fb4c29f378044d7eac3f01815d9966e599841f642d631a
c1ccc(CN(CCc2c[nH]c3ccccc23)Cc2ccccc2)cc1
I-[CH3;D1;+0:1].[c:2]:[c:3]1:[c:4]:[c:5]:[c:6]:[nH;D2;+0:7]:1>>[CH3;D1;+0:1]-[n;H0;D3;+0:7]1:[c:6]:[c:5]:[c:4]:[c:3]:1:[c:2]
89
[{"value": 89.0, "product": "C(C1=CC=CC=C1)N([C@@H](CC1=CN(C2=C(C=C(C=C12)F)F)C)C)CC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
NaH (180 mg of 60% oil dispersion, 4.5 mmol) is added to a solution of dibenzyl-[2-(5,7-difluoro-1H-indol-3-yl)-1(R)-methyl-ethyl]-amine (1.4 g, 3.6 mmol) in 20 ml dimethylformamide under N2 at 0° C. The resulting mixture is stirred for 20 minutes, then is allowed to warm to room temperature over 20 minutes. A 5 ml sol...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1.c1ccccc1.c1ccccc1
HI
CN(C=O)C
null
0.333333
CI.C[C@H](Cc1c[nH]c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1>CN(C=O)C>C[C@H](Cc1cn(C)c2c(F)cc(F)cc12)N(Cc1ccccc1)Cc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-512b38c506b9498185831786eee0d90a
CN(C)C=O.COc1cc2cc[nH]c2cc1F>>COc1cc2c(C=O)c[nH]c2cc1F
COC=1C=C2C=CNC2=CC1F.CN(C=O)C.O=P(Cl)(Cl)Cl.CN(C=O)C.[OH-].[Na+]>>FC1=C(C=C2C(=CNC2=C1)C=O)OC
CN(C)[CH:7]=[O:8].[CH3:1][O:2][c:3]1[cH:4][c:5]2[cH:6][cH:9][nH:10][c:11]2[cH:12][c:13]1[F:14]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([CH:7]=[O:8])[cH:9][nH:10][c:11]2[cH:12][c:13]1[F:14]
CN(C)C=O.COc1cc2cc[nH]c2cc1F
COc1cc2c(C=O)c[nH]c2cc1F
null
null
null
C-C Coupling
OtherReaction
d9ced6f2d1d9464eec389101e666f325da08b904b074a7a40088934efbb18d56
f0bd75a0630092c31f21f61f4a015c77ae0dff14a0b742b4370d7a38fda490f7
c1ccc2[nH]ccc2c1
C-N(-C)-[CH;D2;+0:1]=[O;D1;H0:2].[c:3]:[c:4]1:[#7;a:5]:[c:6]:[cH;D2;+0:7]:[c:8]:1:[c:9]>>[O;D1;H0:2]=[CH;D2;+0:1]-[c;H0;D3;+0:7]1:[c:6]:[#7;a:5]:[c:4](:[c:3]):[c:8]:1:[c:9]
95
[{"value": 95.0, "product": "FC1=C(C=C2C(=CNC2=C1)C=O)OC", "details": "PERCENTYIELD", "is_desired": false}]
10
CELSIUS
15
MINUTE
POCl3 (10.9 ml, 71 mmol) is added dropwise to 21 ml of dimethylformamide under N2 at 10–20° C., is stirred 15 minutes, then a 13 ml dimethylformamide solution of 5-methoxy-6-fluoro-indole (J. Med. Chem., 22:63–69, 1979; 10.7 g, 64.7 mmol) is added at a rate to keep the reaction temperature between 10 and 20° C. After t...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Aldehyde
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
Other
null
10
0.25
CN(C)C=O.COc1cc2cc[nH]c2cc1F>>COc1cc2c(C=O)c[nH]c2cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a2dc7544472245ceae1897b7f180e6d7
CC[N+](=O)[O-].COc1cc2c(C=O)c[nH]c2cc1F>>COc1cc2c(C=C(C)[N+](=O)[O-])c[nH]c2cc1F
[N+](=O)([O-])CC.FC1=C(C=C2C(=CNC2=C1)C=O)OC.C(C)(=O)[O-].[NH4+]>>FC1=C(C=C2C(=CNC2=C1)C=C(C)[N+](=O)[O-])OC
[CH2:8]([CH3:9])[N+:10](=[O:11])[O-:12].O=[CH:7][c:6]1[c:5]2[cH:4][c:3]([O:2][CH3:1])[c:17]([F:18])[cH:16][c:15]2[nH:14][cH:13]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([CH:7]=[C:8]([CH3:9])[N+:10](=[O:11])[O-:12])[cH:13][nH:14][c:15]2[cH:16][c:17]1[F:18]
CC[N+](=O)[O-].COc1cc2c(C=O)c[nH]c2cc1F
COc1cc2c(C=C(C)[N+](=O)[O-])c[nH]c2cc1F
null
null
null
C-C Coupling
OtherReaction
7ede86d40d3d69f429dde089476c8b7ffa9b74bf3050590255e6323d013c2daf
f736727903c0ad5511d468246b8e380897fd19905174c118ffa4ed4d3651f6ea
c1ccc2[nH]ccc2c1
O=[CH;D2;+0:1]-[c:2]1:[c:3]:[#7;a:4]:[c:5]:[c:6]:1.[C;D1;H3:7]-[CH2;D2;+0:8]-[#7;+:9](-[O;-;D1;H0:10])=[O;D1;H0:11]>>[C;D1;H3:7]-[C;H0;D3;+0:8](=[CH;D2;+0:1]-[c:2]1:[c:3]:[#7;a:4]:[c:5]:[c:6]:1)-[#7;+:9](-[O;-;D1;H0:10])=[O;D1;H0:11]
92
[{"value": 92.0, "product": "FC1=C(C=C2C(=CNC2=C1)C=C(C)[N+](=O)[O-])OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.7, "product": "FC1=C(C=C2C(=CNC2=C1)C=C(C)[N+](=O)[O-])OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
3
HOUR
A mixture of nitroethane(44 ml, 611 mmol), 6-fluoro-5-methoxy-1H-indole-3-carbaldehyde (11.8 g, 61 mmol), and ammonium acetate(1.78 g, 23 mmol) is stirred at 100° C. for 3 hours, allowed to cool, and is filtered to give 14 g of 6-fluoro-5-methoxy-3-(2-nitro-propenyl)-1H-indole (92%). Conditions: See reaction.notes.proc...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Nitro group
Enamine
null
null
c1ccc2[nH]ccc2c1
HO-
null
100
3
CC[N+](=O)[O-].COc1cc2c(C=O)c[nH]c2cc1F>>COc1cc2c(C=C(C)[N+](=O)[O-])c[nH]c2cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f7a1ba14ffa947f1be82f724f443f402
N#CCBr.Oc1cccc2[nH]ccc12>>N#CCOc1cccc2[nH]ccc12
BrCC#N.OC1=C2C=CNC2=CC=C1.[H-].[Na+]>>N1C=CC2=C(C=CC=C12)OCC#N
Br[CH2:3][C:2]#[N:1].[OH:4][c:5]1[cH:6][cH:7][cH:8][c:9]2[nH:10][cH:11][cH:12][c:13]12>>[N:1]#[C:2][CH2:3][O:4][c:5]1[cH:6][cH:7][cH:8][c:9]2[nH:10][cH:11][cH:12][c:13]12
N#CCBr.Oc1cccc2[nH]ccc12
N#CCOc1cccc2[nH]ccc12
null
null
CN(C=O)C.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccc2[nH]ccc2c1
Br-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3].[#7;a:4]:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]>>[#7;a:4]:[c:5]:[c:6]:[c:7](-[O;H0;D2;+0:8]-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3]):[c:9]
97
[{"value": 97.0, "product": "N1C=CC2=C(C=CC=C12)OCC#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.8, "product": "N1C=CC2=C(C=CC=C12)OCC#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A 0° C. solution of 4-hydroxyindole (20 g, 150 mmol) in 500 ml of dimethylformamide is treated with NaH (60% dispersion in mineral oil; 6.6 g, 165 mmol). After 30 minutes, bromoacetonitrile (11.5 ml, 165 mmol) is added, and the resulting mixture is allowed to slowly warm to ambient temperature and stir for 3 days. The ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccc2[nH]ccc2c1
HBr
CN(C=O)C.C(C)(=O)OCC
null
0.5
N#CCBr.Oc1cccc2[nH]ccc12>CN(C=O)C.C(C)(=O)OCC>N#CCOc1cccc2[nH]ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7a4c2b57e5d34d249997ab15f038576e
N#CCBr.c1ccc2[nH]ccc2c1>>N#CCn1ccc2ccccc21
BrCC#N.N1C=CC2=CC=CC=C12.[H-].[Na+]>>N1(C=CC2=CC=CC=C12)CC#N
Br[CH2:3][C:2]#[N:1].[nH:4]1[cH:5][cH:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]12>>[N:1]#[C:2][CH2:3][n:4]1[cH:5][cH:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]12
N#CCBr.c1ccc2[nH]ccc2c1
N#CCn1ccc2ccccc21
null
null
CN(C=O)C.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
92cc004fc3e2a92f5c9aa0385cdf93f1126e35d5aa485f4f5fe9240c9543c8fe
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
c1ccc2[nH]ccc2c1
Br-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3].[c:4]:[c:5]1:[c:6]:[c:7]:[c:8]:[nH;D2;+0:9]:1>>[N;D1;H0:3]#[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:9]1:[c:8]:[c:7]:[c:6]:[c:5]:1:[c:4]
27.1
[{"value": 27.0, "product": "N1(C=CC2=CC=CC=C12)CC#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 27.1, "product": "N1(C=CC2=CC=CC=C12)CC#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
A 0° C. solution of indole (7 g, 59.8 mmol) in 200 ml of dimethylformamide is treated with NaH (60% dispersion in mineral oil; 3.1 g, 77.7 mmol). After 20 minutes, bromoacetonitrile (4.2 ml, 59.8 mmol) is added, and the resulting mixture is allowed to slowly warm to ambient temperature and stir overnight. The reaction ...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
HBr
CN(C=O)C.C(C)(=O)OCC
null
0.333333
N#CCBr.c1ccc2[nH]ccc2c1>CN(C=O)C.C(C)(=O)OCC>N#CCn1ccc2ccccc21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a38914c6c46e4909b2e3f31bcb03efa9
CC(C)[N+](=O)[O-].CN(C)CCc1c[nH]c2cccc(F)c12>>CC(C)(Cc1c[nH]c2cccc(F)c12)[N+](=O)[O-]
C(C)(=O)O.FC1=C2C(=CNC2=CC=C1)CCN(C)C.[OH-].[Na+].[N+](=O)([O-])C(C)C>>FC1=C2C(=CNC2=CC=C1)CC(C)([N+](=O)[O-])C
[CH3:1][CH:2]([CH3:3])[N+:15](=[O:16])[O-:17].CN(C)C[CH2:4][c:5]1[cH:6][nH:7][c:8]2[cH:9][cH:10][cH:11][c:12]([F:13])[c:14]12>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[cH:9][cH:10][cH:11][c:12]([F:13])[c:14]12)[N+:15](=[O:16])[O-:17]
CC(C)[N+](=O)[O-].CN(C)CCc1c[nH]c2cccc(F)c12
CC(C)(Cc1c[nH]c2cccc(F)c12)[N+](=O)[O-]
null
null
C(C)(=O)OCC.[Cl-].[Na+].O
C-C Coupling
OtherReaction
410d0ecf550dfec32b5bd37f61aeafc75533d5e4329aa3110c08acb15e21dcaa
fc73a0ba4f6f90cb21df47612bcde105fcd2a049cd56b52924f944fc6a6cbe55
c1ccc2[nH]ccc2c1
C-N(-C)-C-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:1.[C;D1;H3:7]-[CH;D3;+0:8](-[C;D1;H3:9])-[#7;+:10](-[O;-;D1;H0:11])=[O;D1;H0:12]>>[C;D1;H3:7]-[C;H0;D4;+0:8](-[C;D1;H3:9])(-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:1)-[#7;+:10](-[O;-;D1;H0:11])=[O;D1;H0:12]
76
[{"value": 76.0, "product": "FC1=C2C(=CNC2=CC=C1)CC(C)([N+](=O)[O-])C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A slurry of 4-fluoro-3-(dimethylaminoethyl)-1H-indole (4.3 g, 22.4 mmol) in 14.1 ml of 2-nitropropane is treated with solid NaOH (941 mg, 23.5 mmol), and the resulting mixture is heated at reflux overnight. After cooling to ambient temperature, the reaction mixture is acidified with 10%. aqueous acetic acid (25 ml) and...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Tertiary amine
Nitro group
null
null
c1ccc2[nH]ccc2c1
Other
C(C)(=O)OCC.[Cl-].[Na+].O
null
0.5
CC(C)[N+](=O)[O-].CN(C)CCc1c[nH]c2cccc(F)c12>C(C)(=O)OCC.[Cl-].[Na+].O>CC(C)(Cc1c[nH]c2cccc(F)c12)[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c7d2f163f53541348b1ec62b194c7f1c
C=[N+](C)C.COC(=O)c1cccc2[nH]ccc12.[I-]>>COC(=O)c1cccc2[nH]cc(CN(C)C)c12.I
N1C=CC=2C(=CC=CC12)C(=O)OC.C[N+](=C)C.[I-]>>I.COC(=O)C=1C=2C(=CNC2C=CC1)CN(C)C
[CH2:13]=[N+:14]([CH3:15])[CH3:16].[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][c:9]2[nH:10][cH:11][cH:12][c:17]12.[I-:18]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][c:9]2[nH:10][cH:11][c:12]([CH2:13][N:14]([CH3:15])[CH3:16])[c:17]12.[IH:18]
C=[N+](C)C.COC(=O)c1cccc2[nH]ccc12.[I-]
COC(=O)c1cccc2[nH]cc(CN(C)C)c12.I
null
null
C(C)(=O)O
C-C Coupling
OtherReaction
6f78ebae7a6e5f9c15e0d6ab78f58f64a17b670729ecfc39fbb9b9e11c788fae
5c03404e5740858973798689d4be0a8ed62608f5043e578ba3cd6de4363e2dbe
c1ccc2[nH]ccc2c1
[#8:1]-[C:2](=[O;D1;H0:3])-[c:4]:[c:5]1:[cH;D2;+0:6]:[c:7]:[#7;a:8]:[c:9]:1:[c:10].[C;D1;H3:11]-[N+;H0;D3:12](-[C;D1;H3:13])=[CH2;D1;+0:14].[I-;H0;D0:15]>>[#8:1]-[C:2](=[O;D1;H0:3])-[c:4]:[c:5]1:[c:9](:[c:10]):[#7;a:8]:[c:7]:[c;H0;D3;+0:6]:1-[CH2;D2;+0:14]-[N;H0;D3;+0:12](-[C;D1;H3:11])-[C;D1;H3:13].[IH;D0;+0:15]
null
[]
65
CELSIUS
null
null
Methyl indole-4-carboxylate (7.0 g, 40 mmol) and Eschenmoser's salt (N,N-dimethylmethyleneammonium iodide; 7.8 g, 42 mmol) are combined in 130 ml of acetic acid. After heating at 65° C. for 2 hours, the reaction mixture is concentrated in vacuo. The resulting solid is triturated with ethyl acetate, filtered and dried i...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amine
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
null
C(C)(=O)O
65
null
C=[N+](C)C.COC(=O)c1cccc2[nH]ccc12.[I-]>C(C)(=O)O>COC(=O)c1cccc2[nH]cc(CN(C)C)c12.I
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4866853a2f2646d1ab550d48cec29d92
CC(C)[N+](=O)[O-].COC(=O)c1cccc2[nH]cc(CN(C)C)c12>>COC(=O)c1cccc2[nH]cc(CC(C)(C)[N+](=O)[O-])c12
I.COC(=O)C=1C=2C(=CNC2C=CC1)CN(C)C.S(=O)(=O)(OC)OC.C[O-].[Na+].[N+](=O)([O-])C(C)C>>COC(=O)C=1C=2C(=CNC2C=CC1)CC(C)([N+](=O)[O-])C
[CH:14]([CH3:15])([CH3:16])[N+:17](=[O:18])[O-:19].CN(C)[CH2:13][c:12]1[cH:11][nH:10][c:9]2[cH:8][cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[c:20]21>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][c:9]2[nH:10][cH:11][c:12]([CH2:13][C:14]([CH3:15])([CH3:16])[N+:17](=[O:18])[O-:19])[c:20]12
CC(C)[N+](=O)[O-].COC(=O)c1cccc2[nH]cc(CN(C)C)c12
COC(=O)c1cccc2[nH]cc(CC(C)(C)[N+](=O)[O-])c12
null
null
CO.C(C)(=O)OCC.[NH4+].[Cl-]
C-C Coupling
OtherReaction
410d0ecf550dfec32b5bd37f61aeafc75533d5e4329aa3110c08acb15e21dcaa
fc73a0ba4f6f90cb21df47612bcde105fcd2a049cd56b52924f944fc6a6cbe55
c1ccc2[nH]ccc2c1
C-N(-C)-[CH2;D2;+0:1]-[c:2]1:[c:3]:[#7;a:4]:[c:5]:[c:6]:1.[C;D1;H3:7]-[CH;D3;+0:8](-[C;D1;H3:9])-[#7;+:10](-[O;-;D1;H0:11])=[O;D1;H0:12]>>[C;D1;H3:7]-[C;H0;D4;+0:8](-[C;D1;H3:9])(-[CH2;D2;+0:1]-[c:2]1:[c:3]:[#7;a:4]:[c:5]:[c:6]:1)-[#7;+:10](-[O;-;D1;H0:11])=[O;D1;H0:12]
null
[]
null
null
8
HOUR
A 0° C. solution of 3-dimethylaminomethyl-1H-indole-4-carboxylic acid methyl ester hydroiodide (19 g, 52.7 mmol) in 75 ml of methanol and 75 ml of 2-nitropropane is treated with dimethyl sulfate (10 ml, 105.5 mmol) and solid sodium methoxide (6.3 g, 110.6.mmol) sequentially. The resulting mixture is allowed to warm to ...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Tertiary amine
Nitro group
null
null
c1ccc2[nH]ccc2c1
Other
CO.C(C)(=O)OCC.[NH4+].[Cl-]
null
8
CC(C)[N+](=O)[O-].COC(=O)c1cccc2[nH]cc(CN(C)C)c12>CO.C(C)(=O)OCC.[NH4+].[Cl-]>COC(=O)c1cccc2[nH]cc(CC(C)(C)[N+](=O)[O-])c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3dd918785d8c438daa628a564fa5be31
CNC.COC(=O)c1ccc2c(C=O)c[nH]c2c1>>COC(=O)c1ccc2c(N(C)C)cn(C)c2c1.N
[BH4-].[Na+].C(=O)C1=CNC2=CC(=CC=C12)C(=O)OC.CNC.CO>>N.CO.COC(=O)C1=CC=C2C(=CN(C2=C1)C)N(C)C
[NH:12]([CH3:13])[CH3:14].O=[CH:17][c:11]1[c:10]2[cH:9][cH:8][c:7]([C:5]([O:4][CH3:3])=[O:6])[cH:19][c:18]2[nH:16][cH:15]1>>[CH3:3][O:4][C:5](=[O:6])[c:7]1[cH:8][cH:9][c:10]2[c:11]([N:12]([CH3:13])[CH3:14])[cH:15][n:16]([CH3:17])[c:18]2[cH:19]1.[NH3:20]
CNC.COC(=O)c1ccc2c(C=O)c[nH]c2c1
COC(=O)c1ccc2c(N(C)C)cn(C)c2c1.N
null
null
C(Cl)(Cl)Cl.[Cl-].[Na+].O
Heteroatom Alkylation and Arylation
OtherReaction
c7ea80b5fb60b4ece971cabaae8f4e0c032ddb9c0e263eb0712e682a442ca3ff
2d03f38884b1fbb0c0d6e6f2de31afb25102fec87f347c3a123e064c1bfef0ad
c1ccc2[nH]ccc2c1
O=[CH;D2;+0:1]-[c;H0;D3;+0:2]1:[c:3]:[nH;D2;+0:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[C;D1;H3:9]-[NH;D2;+0:10]-[C;D1;H3:11]>>[C;D1;H3:9]-[N;H0;D3;+0:10](-[C;D1;H3:11])-[c;H0;D3;+0:2]1:[c:3]:[n;H0;D3;+0:4](-[CH3;D1;+0:1]):[c:5](:[c:6]):[c:7]:1:[c:8]
99
[{"value": 20.0, "product": "N.CO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.0, "product": "COC(=O)C1=CC=C2C(=CN(C2=C1)C)N(C)C", "details": "PERCENTYIELD", "is_desired": false}]
55
CELSIUS
45
MINUTE
A solution of methyl 3-formylindole-6-carboxylate (8.0 g, 39.3 mmol) in 270 ml methanol is treated with dimethylamine (40% aqueous; 267 ml, 2.56 mol) at ambient temperature. After 45 minutes, NaBH4 (4.45 g, 118.1 mmol) is added, and the resulting mixture is heated at 55° C. for 3 hours. The reaction mixture is allowed ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine
Tertiary amine
c1ccc2[nH]ccc2c1
c1ccc2cc[nH]c2c1
c1ccc2cc[nH]c2c1
null
C(Cl)(Cl)Cl.[Cl-].[Na+].O
55
0.75
CNC.COC(=O)c1ccc2c(C=O)c[nH]c2c1>C(Cl)(Cl)Cl.[Cl-].[Na+].O>COC(=O)c1ccc2c(N(C)C)cn(C)c2c1.N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-862fad865d5d4554aecfa4b466bec1e1
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.COC(=O)CCl>>COCOC(=O)c1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)O)(C)C)=O.CN(C=O)C.[H-].[Na+].COC(CCl)=O>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C(=O)OCOC)(C)C)=O
[OH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([CH2:13][C:14]([CH3:15])([CH3:16])[NH:17][C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[cH:25][nH:26][c:27]12.ClC[C:3]([O:2][CH3:1])=[O:4]>>[CH3:1][O:2][CH2:3][O:4][C:5](=[O:6])[c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([CH2:13][C:14]([CH3:15])([CH3:16])[NH:17][C:18](=...
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.COC(=O)CCl
COCOC(=O)c1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
null
null
null
Acylation
OtherReaction
462f2ec62d81e992577a968a9b12fce9fe1090236ae6c9f8b084f1cedb24cddd
5e9e0b01f8c9a1c10ac2bdfadca2d4bb3d9d0593654f2be0a33adb4d01012cf3
c1ccc2[nH]ccc2c1
Cl-C-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[#8:3]-[C;D1;H3:4].[OH;D1;+0:5]-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]>>[C;D1;H3:4]-[#8:3]-[CH2;D2;+0:1]-[O;H0;D2;+0:2]-[C:13](=[O;H0;D1;+0:5])-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](:[c:10]):[#7;a:11]:[c:12]
30
[{"value": 30.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C(=O)OCOC)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
15
HOUR
A solution of [2-(7-hydroxy-1H-indol-3-yl)-1,1-dimethyl-ethyl]-carbamic acid tert-butyl ester (609 mg, 2.0 mmol) is dissolved in dry dimethylformamide (30 ml) under a nitrogen atmosphere and treated with sodium hydride (84 mg, 2.1 mmol, 60% dispersion in oil) added portion-wise over a 10 minute period. The mixture is c...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Aromatic alcohol
Ester
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
HCl
null
null
15
CC(C)(Cc1c[nH]c2c(O)cccc12)NC(=O)OC(C)(C)C.COC(=O)CCl>>COCOC(=O)c1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d6abe5dd3fb941639e55b4abc3d4079d
COCOC(=O)c1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12.CS(N)(=O)=O>>CC(C)(Cc1c[nH]c2c(C(=O)OCNS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C(=O)OCOC)(C)C)=O.CS(=O)(=O)N.C[Al](C)C>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C(=O)OCNS(=O)(=O)C)(C)C)=O
CO[CH2:13][O:12][C:10]([c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:23][C:24](=[O:25])[O:26][C:27]([CH3:28])([CH3:29])[CH3:30])[c:22]2[cH:21][cH:20][cH:19]1)=[O:11].[NH2:14][S:15]([CH3:16])(=[O:17])=[O:18]>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([C:10](=[O:11])[O:12][CH2:13][NH:14...
COCOC(=O)c1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12.CS(N)(=O)=O
CC(C)(Cc1c[nH]c2c(C(=O)OCNS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
null
null
ClCCl
Heteroatom Alkylation and Arylation
OtherReaction
27d6bcdad0878087216dc40eea1f1f35fccd29dfa60fe8ed3aa664fae6aef29b
0d14747908d603e8fc04aed79bbcb75d879874eb9fb49385d2afe908ed402dd8
c1ccc2[nH]ccc2c1
C-O-[CH2;D2;+0:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[c:5]:[c:6]:[#7;a:7].[C;D1;H3:8]-[#16:9](-[NH2;D1;+0:10])(=[O;D1;H0:11])=[O;D1;H0:12]>>[#7;a:7]:[c:6]:[c:5]-[C:3](=[O;D1;H0:4])-[#8:2]-[CH2;D2;+0:1]-[NH;D2;+0:10]-[#16:9](-[C;D1;H3:8])(=[O;D1;H0:11])=[O;D1;H0:12]
117.8
[{"value": 90.0, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C(=O)OCNS(=O)(=O)C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 117.8, "product": "C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C(=O)OCNS(=O)(=O)C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of methanesulfonamide (106 mg, 1.12 mmol) and trimethyl aluminum (2.0 M in hexanes, 0.56 ml, 1.12 mmol) in dry dichloromethane (5.0 ml) is stirred at room temperature under a nitrogen atmosphere for 20 minutes. A solution of [2-(7-(methoxycarbomethoxy)-1H-indol-3-yl)-1,1-dimethyl-ethyl]-carbamic acid tert-bu...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Ester.Ether
Sulfonamide.Ester
null
null
c1ccc2[nH]ccc2c1
HO-
ClCCl
null
null
COCOC(=O)c1cccc2c(CC(C)(C)NC(=O)OC(C)(C)C)c[nH]c12.CS(N)(=O)=O>ClCCl>CC(C)(Cc1c[nH]c2c(C(=O)OCNS(C)(=O)=O)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e00e490317614dde964f7b2a9f8b6a90
C=Cc1ccc(C#N)cc1.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=Cc3ccc(C#N)cc3)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CS(=O)(=O)C(F)(F)F)(C)C)=O.C(#N)C1=CC=C(C=C)C=C1>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C=CC1=CC=C(C=C1)C#N)(C)C)=O
C=[CH:11][c:12]1[cH:13][cH:14][c:15]([C:16]#[N:17])[cH:18][cH:19]1.O=S(=O)(C(F)(F)F)[CH2:10][c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:24][C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31])[c:23]2[cH:22][cH:21][cH:20]1>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([CH:10]=[CH:11]...
C=Cc1ccc(C#N)cc1.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C
CC(C)(Cc1c[nH]c2c(C=Cc3ccc(C#N)cc3)cccc12)NC(=O)OC(C)(C)C
null
null
null
C-C Coupling
OtherReaction
be72368e485bae2cf3a6c9f3c288e958fb19cb924e46b869d59552ae07869be9
9a367fc6597a2c2d2ef687b5d530f141dc98e4ffcb30f47f73afa833e2c55025
C(=Cc1cccc2cc[nH]c12)c1ccccc1
C=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].F-C(-F)(-F)-S(=O)(=O)-[CH2;D2;+0:5]-[c:6](:[c:7]):[c:8](:[c:9]):[#7;a:10]:[c:11]>>[c:3]:[c:2](-[CH;D2;+0:1]=[CH;D2;+0:5]-[c:6](:[c:7]):[c:8](:[c:9]):[#7;a:10]:[c:11]):[c:4]
null
[]
null
null
null
null
(2-{7-[2-(4-Cyano-phenyl)-vinyl]-1H-indol-3-yl}-1,1-dimethyl-ethyl)-carbamic acid tert-butyl ester is prepared from [1,1-dimethyl-2-(7-trifluoromethanesulfonylmethyl-1H-indol-3-yl)-ethyl]-carbamic acid tert-butyl ester and 4-cyanostyrene as described for the preparation of Amine 23 (93%). FDMS m/e=315.2 (M++1). Conditi...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Sulfone.Vinyl
null
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
HF
null
null
null
C=Cc1ccc(C#N)cc1.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=Cc3ccc(C#N)cc3)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-91930206a1db4b719ea533076ef50a06
C=Cc1cnccn1.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=Cc3cnccn3)cccc12)NC(=O)OC(C)(C)C
C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)CS(=O)(=O)C(F)(F)F)(C)C)=O.C(=C)C1=NC=CN=C1>>C(C)(C)(C)OC(NC(CC1=CNC2=C(C=CC=C12)C=CC1=NC=CN=C1)(C)C)=O
[CH2:10]=[CH:11][c:12]1[cH:13][n:14][cH:15][cH:16][n:17]1.O=S(=O)(C[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[NH:22][C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29])[c:21]2[cH:20][cH:19][cH:18]1)C(F)(F)F>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([CH:10]=[CH:11][c:12]3[cH:13][n...
C=Cc1cnccn1.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C
CC(C)(Cc1c[nH]c2c(C=Cc3cnccn3)cccc12)NC(=O)OC(C)(C)C
null
null
null
C-C Coupling
OtherReaction
9ee5c848b3529c0571d068ce5ea5cd4d1d3705da2182d3214d2c9187dbcdd8d9
9a367fc6597a2c2d2ef687b5d530f141dc98e4ffcb30f47f73afa833e2c55025
C(=Cc1cccc2cc[nH]c12)c1cnccn1
F-C(-F)(-F)-S(=O)(=O)-C-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].[#7;a:8]:[c:9]:[c:10](-[C:11]=[CH2;D1;+0:12]):[#7;a:13]>>[#7;a:8]:[c:9]:[c:10](-[C:11]=[CH;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]):[#7;a:13]
null
[]
null
null
null
null
{1,1-Dimethyl-2-[7-(2-pyrazin-2-yl-vinyl)-1H-indol-3-yl]-ethyl}-carbamic acid tert-butyl ester is prepared from [1,1-dimethyl-2-(7-trifluoromethanesulfonylmethyl-1H-indol-3-yl)-ethyl]-carbamic acid tert-butyl ester and 2-vinylpyrazine as described for the preparation of Amine 23 (99%). FDMS m/e=393.2 (M++1) Conditions:...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Sulfone.Vinyl
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1cnccn1.c1ccc2[nH]ccc2c1
HF
null
null
null
C=Cc1cnccn1.CC(C)(Cc1c[nH]c2c(CS(=O)(=O)C(F)(F)F)cccc12)NC(=O)OC(C)(C)C>>CC(C)(Cc1c[nH]c2c(C=Cc3cnccn3)cccc12)NC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8866daba5bfc47cba6e2aaa9a9e6d8c6
CN(C)Cc1c[nH]c2c([N+](=O)[O-])cccc12.COS(=O)(=O)OC>>CC(C)(Cc1c[nH]c2c([N+](=O)[O-])cccc12)[N+](=O)[O-]
CN(C)CC1=CNC2=C1C=CC=C2[N+](=O)[O-].COS(=O)(=O)OC.C[O-].[Na+]>>[N+](=O)([O-])C(CC1=CNC2=C(C=CC=C12)[N+](=O)[O-])(C)C
[CH3:2][N:17]([CH3:3])[CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([N+:10](=[O:11])[O-:12])[cH:13][cH:14][cH:15][c:16]12.COS(=O)(=[O:18])[O:19][CH3:1]>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([N+:10](=[O:11])[O-:12])[cH:13][cH:14][cH:15][c:16]12)[N+:17](=[O:18])[O-:19]
CN(C)Cc1c[nH]c2c([N+](=O)[O-])cccc12.COS(=O)(=O)OC
CC(C)(Cc1c[nH]c2c([N+](=O)[O-])cccc12)[N+](=O)[O-]
null
null
CO.[N+](=O)([O-])C(C)C
Functional Group Addition
OtherReaction
5bd93d2f1982c88e84b5fc5292e57c4ade933d319b1c969f1bcf720de5d2b688
bfdf996aa8a01161a3995460dbc607f36b6b31262f523474e587d94418778376
c1ccc2[nH]ccc2c1
C-O-S(=O)(=[O;H0;D1;+0:1])-[O;H0;D2;+0:2]-[CH3;D1;+0:3].[CH3;D1;+0:4]-[N;H0;D3;+0:5](-[CH3;D1;+0:6])-[CH2;D2;+0:7]-[c:8]1:[c:9]:[c:10]:[#7;a:11]:[c:12]:1>>[CH3;D1;+0:3]-[C;H0;D4;+0:4](-[CH3;D1;+0:6])(-[CH2;D2;+0:7]-[c:8]1:[c:9]:[c:10]:[#7;a:11]:[c:12]:1)-[N+;H0;D3:5](-[O-;H0;D1:2])=[O;H0;D1;+0:1]
131
[{"value": 69.0, "product": "[N+](=O)([O-])C(CC1=CNC2=C(C=CC=C12)[N+](=O)[O-])(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 131.0, "product": "[N+](=O)([O-])C(CC1=CNC2=C(C=CC=C12)[N+](=O)[O-])(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
The 7-nitrogramine salt (2.0 g, 5.8 mmol) is suspended in a mixture of 2-nitropropane (9.5 mL) and methanol (9.5 mL). Dimethylsulfate (1.09 mL, 11.5 mmol) is added dropwise via syringe, and the resulting yellow solution is stirred at room temperature for 5 minutes. Sodium methoxide (0.62 g, 11.5 mmol) is then added in ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Nitro group
null
null
c1ccc2[nH]ccc2c1
HO-
CO.[N+](=O)([O-])C(C)C
null
0.083333
CN(C)Cc1c[nH]c2c([N+](=O)[O-])cccc12.COS(=O)(=O)OC>CO.[N+](=O)([O-])C(C)C>CC(C)(Cc1c[nH]c2c([N+](=O)[O-])cccc12)[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fcc97bd77b3c4880aa5eed15a29d7d18
CC(C)(Cc1c[nH]c2c([N+](=O)[O-])cccc12)[N+](=O)[O-].O=S(=O)(Cl)c1ccccc1>>CC(C)(Cc1c[nH]c2c(NS(=O)(=O)c3ccccc3)cccc12)[N+](=O)[O-]
[N+](=O)([O-])C(CC1=CNC2=C(C=CC=C12)[N+](=O)[O-])(C)C.[N+](=O)([O-])C(CC1=CNC2=C(C=CC=C12)[N+](=O)[O-])(C)C.C1(=CC=CC=C1)S(=O)(=O)Cl>>[N+](=O)([O-])C(CC1=CNC2=C(C=CC=C12)NS(=O)(=O)C1=CC=CC=C1)(C)C
O=[N+:10]([O-])[c:9]1[c:8]2[nH:7][cH:6][c:5]([CH2:4][C:2]([CH3:1])([CH3:3])[N+:24](=[O:25])[O-:26])[c:23]2[cH:22][cH:21][cH:20]1.Cl[S:11](=[O:12])(=[O:13])[c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1>>[CH3:1][C:2]([CH3:3])([CH2:4][c:5]1[cH:6][nH:7][c:8]2[c:9]([NH:10][S:11](=[O:12])(=[O:13])[c:14]3[cH:15][cH:16][cH:17][c...
CC(C)(Cc1c[nH]c2c([N+](=O)[O-])cccc12)[N+](=O)[O-].O=S(=O)(Cl)c1ccccc1
CC(C)(Cc1c[nH]c2c(NS(=O)(=O)c3ccccc3)cccc12)[N+](=O)[O-]
null
[Pd]
C(C)(=O)OCC.N1=CC=CC=C1
Acylation
OtherReaction
6d82f556414835bcf6b9f0bce649a05d5bc17ae300992ec18a68cb9f62c221e6
8cfa256053695afc670cfb6cc03c2a6ebab576dbef684fdcb26ee84d655f5de5
O=S(=O)(Nc1cccc2cc[nH]c12)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].O=[N+;H0;D3:7](-[O-])-[c:8](:[c:9]):[c:10](:[c:11]):[#7;a:12]:[c:13]>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10](:[c:11]):[#7;a:12]:[c:13])-[c:4](:[c:5]):[c:6]
71
[{"value": 71.0, "product": "[N+](=O)([O-])C(CC1=CNC2=C(C=CC=C12)NS(=O)(=O)C1=CC=CC=C1)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
3-(2-Nitro-2-methylpropyl)-7-nitroindole (1.89 g, 7.2 mmol) is dissolved in ethyl acetate (75 mL) and 10% Pd/C is added (750 mg). The mixture is stirred under a balloon of nitrogen for 2–3 hours. The mixture is filtered to remove the Pd/C, and the filtrate is evaporated to give a crude oil. This crude 3-(2-nitro-2-meth...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Sulfonyl halide
Sulfonamide
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
Other
[Pd].C(C)(=O)OCC.N1=CC=CC=C1
0
null
CC(C)(Cc1c[nH]c2c([N+](=O)[O-])cccc12)[N+](=O)[O-].O=S(=O)(Cl)c1ccccc1>[Pd].C(C)(=O)OCC.N1=CC=CC=C1>CC(C)(Cc1c[nH]c2c(NS(=O)(=O)c3ccccc3)cccc12)[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-408263d2ae6444428752aab62ae17bb3
CCOC(=O)CCCCN(CCc1cc(F)ccc1OC)Cc1ccc(C(=O)OC)cc1>>COC(=O)CCCCN(CCc1cc(F)ccc1O)Cc1ccc(C(=O)OC)cc1
CO.B(Br)(Br)Br.C(C)OC(CCCCN(CCC1=C(C=CC(=C1)F)OC)CC1=CC=C(C(=O)OC)C=C1)=O>>COC(CCCCN(CCC1=C(C=CC(=C1)F)O)CC1=CC=C(C(=O)OC)C=C1)=O
C[CH2:1][O:2][C:3](=[O:4])[CH2:5][CH2:6][CH2:7][CH2:8][N:9]([CH2:10][CH2:11][c:12]1[cH:13][c:14]([F:15])[cH:16][cH:17][c:18]1[O:19]C)[CH2:20][c:21]1[cH:22][cH:23][c:24]([C:25](=[O:26])[O:27][CH3:28])[cH:29][cH:30]1>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][CH2:6][CH2:7][CH2:8][N:9]([CH2:10][CH2:11][c:12]1[cH:13][c:14]([F:15])[...
CCOC(=O)CCCCN(CCc1cc(F)ccc1OC)Cc1ccc(C(=O)OC)cc1
COC(=O)CCCCN(CCc1cc(F)ccc1O)Cc1ccc(C(=O)OC)cc1
null
null
ClCCl
Deprotection
OtherReaction
f59b8116b9a9ca99fb99fbc349fd2f3ba7a407b5d14f87b4825067d0befd0c68
e00f9a9e80835d92a5562f8e4d77c15ee40726b40cd6dcf858e9b9fabcbd50cd
c1ccc(CCNCc2ccccc2)cc1
C-[CH2;D2;+0:1]-[#8:2]-[C:3](-[C:4])=[O;D1;H0:5].C-[O;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:4]-[C:3](=[O;D1;H0:5])-[#8:2]-[CH3;D1;+0:1].[OH;D1;+0:6]-[c:7](:[c:8]):[c:9]
null
[]
0
CELSIUS
1
HOUR
2.6 g (5.84 mmol) of methyl 4-({(5-ethoxy-5-oxopentyl)[2-(5-fluoro-2-methoxy-phenyl)ethyl]amino}methyl)benzoate are dissolved in 50 ml of dichloromethane, the mixture is cooled to 0° C., and 19.3 ml (19.3 mmol) of a 1N solution of boron tribromide in dichloromethane are added dropwise. The solution is stirred at 0° C. ...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether
Ester.Aromatic alcohol
null
null
c1ccccc1.c1ccccc1
Other
ClCCl
0
1
CCOC(=O)CCCCN(CCc1cc(F)ccc1OC)Cc1ccc(C(=O)OC)cc1>ClCCl>COC(=O)CCCCN(CCc1cc(F)ccc1O)Cc1ccc(C(=O)OC)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-04c146a1b0024307add260bad868c423
COC(=O)CCCCN(CCc1ccccc1OCc1ccccc1Cl)Cc1ccc(C(=O)OC)cc1>>O=C(O)CCCCN(CCc1ccccc1OCc1ccccc1Cl)Cc1ccc(C(=O)O)cc1
ClC1=C(COC2=C(CCN(CCCCC(=O)OC)CC3=CC=C(C(=O)OC)C=C3)C=CC=C2)C=CC=C1.O.[OH-].[Na+]>>C(=O)(O)CCCCN(CCC1=C(C=CC=C1)OCC1=C(C=CC=C1)Cl)CC1=CC=C(C(=O)O)C=C1
C[O:3][C:2](=[O:1])[CH2:4][CH2:5][CH2:6][CH2:7][N:8]([CH2:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][c:16]1[O:17][CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23][c:24]1[Cl:25])[CH2:26][c:27]1[cH:28][cH:29][c:30]([C:31](=[O:32])[O:33]C)[cH:34][cH:35]1>>[O:1]=[C:2]([OH:3])[CH2:4][CH2:5][CH2:6][CH2:7][N:8]([CH2:9][CH2:10][c...
COC(=O)CCCCN(CCc1ccccc1OCc1ccccc1Cl)Cc1ccc(C(=O)OC)cc1
O=C(O)CCCCN(CCc1ccccc1OCc1ccccc1Cl)Cc1ccc(C(=O)O)cc1
null
null
CO
Deprotection
OtherReaction
6e62db7aac546f574bcfb83067ba8906c30fcbfedfc37aa16b5eaad33833f45a
ed5fed81ba501ef41c88831ec6b9463b899bfdd0815c4145ae51c79addb226d0
c1ccc(CNCCc2ccccc2OCc2ccccc2)cc1
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].C-[O;H0;D2;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1].[O;D1;H0:7]=[C:6](-[OH;D1;+0:5])-[c:8]
null
[]
60
CELSIUS
1
HOUR
124.8 mg (0.238 mmol) of methyl 4-{[{2-[(2-chlorobenzyl)-oxy]phenethyl}(5-methoxy-5-oxopentyl)amino]methyl}benzoate from Ex. 1 are initially charged in 0.3 ml of methanol and 0.17 ml of water and admixed with 0.2 ml of a 40% strength sodium hydroxide solution. The mixture is stirred at 60° C. for one hour and then cool...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Carboxylic acid.Carboxylic acid
null
null
c1ccccc1.c1ccccc1.c1ccccc1
Other
CO
60
1
COC(=O)CCCCN(CCc1ccccc1OCc1ccccc1Cl)Cc1ccc(C(=O)OC)cc1>CO>O=C(O)CCCCN(CCc1ccccc1OCc1ccccc1Cl)Cc1ccc(C(=O)O)cc1