dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
time_units
large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f63e52fc4e484a91b3e232e390750d6f
CC#N.Nc1ncc(Br)cc1[N+](=O)[O-]>>N#Cc1ncc(Br)cc1[N+](=O)[O-]
NC1=NC=C(C=C1[N+](=O)[O-])Br.C(C)(C)(C)ON=O.C(C)#N>>BrC=1C=C(C(=NC1)C#N)[N+](=O)[O-]
C[C:2]#[N:1].N[c:3]1[n:4][cH:5][c:6]([Br:7])[cH:8][c:9]1[N+:10](=[O:11])[O-:12]>>[N:1]#[C:2][c:3]1[n:4][cH:5][c:6]([Br:7])[cH:8][c:9]1[N+:10](=[O:11])[O-:12]
CC#N.Nc1ncc(Br)cc1[N+](=O)[O-]
N#Cc1ncc(Br)cc1[N+](=O)[O-]
null
null
null
C-C Coupling
OtherReaction
7be32428aabd580dfbed2e434f7904a98f0e54bc30b8b5f4dba0a6d14252e209
5270ba81df65d040f7a2858a28254c13e4f1fb0313393de6d45aa339bf5619bd
c1ccncc1
C-[C;H0;D2;+0:1]#[N;D1;H0:2].N-[c;H0;D3;+0:3](:[#7;a:4]:[c:5]):[c:6](-[#7;+:7]):[c:8]>>[#7;+:7]-[c:6](:[c:8]):[c;H0;D3;+0:3](-[C;H0;D2;+0:1]#[N;D1;H0:2]):[#7;a:4]:[c:5]
41
[{"value": 41.0, "product": "BrC=1C=C(C(=NC1)C#N)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Heat a solution of 2-amino-5-bromo-3-nitropyridine (2.18 g, 10 mmol), cuprous cyanide (1.33 g, 15 mmol) and tert-butylnitrite (2.0 mL, 15 mmol) in acetonitrile (50 mL) at 60° C. for 2 hours. Cool the solution and partitioned between ethyl acetate (100 mL) and saturated aqueous NaHCO3 (100 mL). Extract the aqueous layer...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Primary amine
Nitrile
c1ccncc1
c1ccncc1
c1ccncc1
Other
null
null
null
CC#N.Nc1ncc(Br)cc1[N+](=O)[O-]>>N#Cc1ncc(Br)cc1[N+](=O)[O-]
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5b19e67aa6484aacaa880438d505242b
Cc1cccn[c]1[Zn+].N#Cc1ncc(Br)cc1[N+](=O)[O-]>>Cc1cccnc1-c1cnc(C#N)c([N+](=O)[O-])c1
BrC=1C=C(C(=NC1)C#N)[N+](=O)[O-].[Br-].CC=1C(=NC=CC1)[Zn+]>>CC=1C(=NC=CC1)C=1C=C(C(=NC1)C#N)[N+](=O)[O-]
[Zn+][c:7]1[c:2]([CH3:1])[cH:3][cH:4][cH:5][n:6]1.Br[c:8]1[cH:9][n:10][c:11]([C:12]#[N:13])[c:14]([N+:15](=[O:16])[O-:17])[cH:18]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1-[c:8]1[cH:9][n:10][c:11]([C:12]#[N:13])[c:14]([N+:15](=[O:16])[O-:17])[cH:18]1
Cc1cccn[c]1[Zn+].N#Cc1ncc(Br)cc1[N+](=O)[O-]
Cc1cccnc1-c1cnc(C#N)c([N+](=O)[O-])c1
null
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1
C1CCOC1
C-C Coupling
OtherReaction
e4ecd4c8f01d2effb96acd4b7efc6dcca828274ea1bedd77506f1b8e3573c914
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1ccc(-c2cccnc2)nc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1.[C;D1;H3:7]-[c:8](:[c:9]):[c;H0;D3;+0:10](-[Zn+]):[#7;a:11]:[c:12]>>[C;D1;H3:7]-[c:8](:[c:9]):[c;H0;D3;+0:10](-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1):[#7;a:11]:[c:12]
88
[{"value": 88.0, "product": "CC=1C(=NC=CC1)C=1C=C(C(=NC1)C#N)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.8, "product": "CC=1C(=NC=CC1)C=1C=C(C(=NC1)C#N)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Heat a solution of 5-bromo-3-nitropyridine-2-carbonitrile (228 mg, 1.0 mmol), tetrakis(triphenylphosphine)palladium(0) (15 mg), 3-methyl-2-pyridylzinc bromide (0.5 M in THF, 3 mL, 1.5 mmol) in THF (5 mL) at 60° C. for 2 hours. Cool the solution and partition between ethyl acetate (10 mL) and saturated aqueous NaHCO3 (1...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccncc1.c1ccncc1
c1ccncc1.c1ccncc1
c1ccncc1.c1ccncc1
Br-.Zn
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.C1CCOC1
null
null
Cc1cccn[c]1[Zn+].N#Cc1ncc(Br)cc1[N+](=O)[O-]>C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.C1CCOC1>Cc1cccnc1-c1cnc(C#N)c([N+](=O)[O-])c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1ec110cfd6604b6995af219e708ec667
Cc1cccnc1-c1cnc(C#N)c([N+](=O)[O-])c1>>Cc1cccnc1-c1cnc(C(N)=O)c(N)c1
CC=1C(=NC=CC1)C=1C=C(C(=NC1)C#N)[N+](=O)[O-].[Cl-].[Ca+2].[Cl-].C(C)O>>NC=1C(=NC=C(C1)C1=NC=CC=C1C)C(=O)N
[O-][N+:16](=[O:14])[c:15]1[c:11]([C:12]#[N:13])[n:10][cH:9][c:8](-[c:7]2[c:2]([CH3:1])[cH:3][cH:4][cH:5][n:6]2)[cH:17]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1-[c:8]1[cH:9][n:10][c:11]([C:12]([NH2:13])=[O:14])[c:15]([NH2:16])[cH:17]1
Cc1cccnc1-c1cnc(C#N)c([N+](=O)[O-])c1
Cc1cccnc1-c1cnc(C(N)=O)c(N)c1
null
[Fe]
O
Functional Group Interconversion
OtherReaction
ede7d2a6ee11f3b3697b1dfb480a8f492854589e148f2058b38ac2e2cd797a36
cb5481c22f68622a17796d4a172dd074a4fb2bd7f9c138bcaa93b97fc12e084f
c1ccc(-c2cccnc2)nc1
[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[#7;a:4]:[c:5]):[c:6](-[N+;H0;D3:7](-[O-])=[O;H0;D1;+0:8]):[c:9]>>[NH2;D1;+0:1]-[C;H0;D3;+0:2](=[O;H0;D1;+0:8])-[c:3](:[#7;a:4]:[c:5]):[c:6](-[NH2;D1;+0:7]):[c:9]
94
[{"value": 94.0, "product": "NC=1C(=NC=C(C1)C1=NC=CC=C1C)C(=O)N", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Heat a solution of 5-(3-methyl(2-pyridyl))-3-nitropyridine-2-carbonitrile (1 g, 4.1 mmol), iron (2.3 g, 40 mmol) and calcium chloride (560 mg, 5 mmol) in ethanol (15 mL) and water (4 mL) to reflux for 1 hour. Cool the mixture, filter through Celite and wash with ethyl acetate. Evaporate the filtrate and re-dissolve the...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Nitro group
Primary amide.Primary amine
null
null
c1ccncc1.c1ccncc1
Other
[Fe].O
null
null
Cc1cccnc1-c1cnc(C#N)c([N+](=O)[O-])c1>[Fe].O>Cc1cccnc1-c1cnc(C(N)=O)c(N)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0d541d70246742768408266a370c8bc3
COCc1nc2cc(-c3ncccc3C(F)(F)F)cnc2c(=O)[nH]1.O=P(Cl)(Cl)Cl>>COCc1nc(Cl)c2ncc(-c3ncccc3C(F)(F)F)cc2n1
P(=O)(Cl)(Cl)Cl.FC(C=1C(=NC=CC1)C1=CC=2N=C(NC(C2N=C1)=O)COC)(F)F.N1=C(C=CC=C1C)C>>ClC=1C2=C(N=C(N1)COC)C=C(C=N2)C2=NC=CC=C2C(F)(F)F
O=[c:6]1[nH:5][c:4]([CH2:3][O:2][CH3:1])[n:24][c:23]2[c:8]1[n:9][cH:10][c:11](-[c:12]1[n:13][cH:14][cH:15][cH:16][c:17]1[C:18]([F:19])([F:20])[F:21])[cH:22]2.O=P(Cl)(Cl)[Cl:7]>>[CH3:1][O:2][CH2:3][c:4]1[n:5][c:6]([Cl:7])[c:8]2[n:9][cH:10][c:11](-[c:12]3[n:13][cH:14][cH:15][cH:16][c:17]3[C:18]([F:19])([F:20])[F:21])[cH:...
COCc1nc2cc(-c3ncccc3C(F)(F)F)cnc2c(=O)[nH]1.O=P(Cl)(Cl)Cl
COCc1nc(Cl)c2ncc(-c3ncccc3C(F)(F)F)cc2n1
null
null
C(Cl)(Cl)Cl
Functional Group Interconversion
OtherReaction
333a0516a9bcf357e640bc314ff77fe9ec1320c775bca1158466fec62a1bdede
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc(-c2cnc3cncnc3c2)nc1
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].O=[c;H0;D3;+0:2]1:[nH;D2;+0:3]:[c:4](-[C:5]):[#7;a:6]:[c:7](:[c:8]):[c:9]:1:[#7;a:10]:[c:11]>>[C:5]-[c:4]1:[#7;a:6]:[c:7](:[c:8]):[c:9](:[#7;a:10]:[c:11]):[c;H0;D3;+0:2](-[Cl;H0;D1;+0:1]):[n;H0;D2;+0:3]:1
null
[]
null
null
null
null
Dissolve 7-(3-trifluoromethyl-pyridin-2-yl)-2-methoxymethyl-3H-pyrido[3,2-d]pyrimidin-4-one (276 mg, 0.822 mmol) in CHCl3 (25 mL) and 2,6-lutidine (294 mg, 2.74 mmol). Add phosphorous oxycloride (0.255 mL, 2.74 mmol) dropwise and heat the resulting solution to reflux for 24 hours. Cool the solution and remove the solve...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1cnc2cncnc2c1
c1cnc2cncnc2c1
c1cnc2cncnc2c1.c1ccncc1
HCl
C(Cl)(Cl)Cl
null
null
COCc1nc2cc(-c3ncccc3C(F)(F)F)cnc2c(=O)[nH]1.O=P(Cl)(Cl)Cl>C(Cl)(Cl)Cl>COCc1nc(Cl)c2ncc(-c3ncccc3C(F)(F)F)cc2n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9baff1f9762947f78bec357af27b36b8
CCOCC.N#Cc1ncccc1Cl>>CC(=O)c1ncccc1Cl
ClC=1C(=NC=CC1)C#N.C1CCOC1.C(C)OCC.Cl>>C(C)(=O)C1=NC=CC=C1Cl
CC[O:3]C[CH3:1].N#[C:2][c:4]1[n:5][cH:6][cH:7][cH:8][c:9]1[Cl:10]>>[CH3:1][C:2](=[O:3])[c:4]1[n:5][cH:6][cH:7][cH:8][c:9]1[Cl:10]
CCOCC.N#Cc1ncccc1Cl
CC(=O)c1ncccc1Cl
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
643b9d210906c1df38fa997852698e729d0316bdb35f50266fb1b09ae476eb8e
a7c966337c9a564ffde7cdff914cb3598adf1a30626c7d972cd5f8fafc6bcb42
c1ccncc1
C-C-[O;H0;D2;+0:1]-C-[CH3;D1;+0:2].N#[C;H0;D2;+0:3]-[c:4](:[c:5]):[#7;a:6]:[c:7]>>[CH3;D1;+0:2]-[C;H0;D3;+0:3](=[O;H0;D1;+0:1])-[c:4](:[c:5]):[#7;a:6]:[c:7]
null
[]
null
null
2
HOUR
Dissolve 3-chloro-2-cyanopyridine (10.0 g, 0.072 mol, Chem. Pharm. Bull. (1985) 33:565-571) in anhydrous THF (200 mL) under N2 atmosphere and cool in an ice bath. Add drop wise 3.0 M MeMgl in diethyl ether (48 ml, 0.14 mol) to the reaction mixture and stir in an ice bath for 2 hours. Pour the reaction mixture over ice ...
10.6084/m9.figshare.5104873.v1
null
Ether.Nitrile
Ketone
null
null
c1ccncc1
Other
null
null
2
CCOCC.N#Cc1ncccc1Cl>>CC(=O)c1ncccc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0ceca5cd1c6a4e9aa6e737c0719f58ab
COCC(=O)Cl.NC(=O)c1ccc(-c2ncccc2Cl)nc1N>>COCc1nc2nc(-c3ncccc3Cl)ccc2c(=O)[nH]1
[OH-].[Na+].N1=CC=CC=C1.COCC(=O)Cl.NC1=C(C=CC(=N1)C1=NC=CC=C1Cl)C(=O)N>>ClC=1C(=NC=CC1)C=1C=CC2=C(N=C(NC2=O)COC)N1
O=[C:4](Cl)[CH2:3][O:2][CH3:1].[NH2:5][c:6]1[n:7][c:8](-[c:9]2[n:10][cH:11][cH:12][cH:13][c:14]2[Cl:15])[cH:16][cH:17][c:18]1[C:19](=[O:20])[NH2:21]>>[CH3:1][O:2][CH2:3][c:4]1[n:5][c:6]2[n:7][c:8](-[c:9]3[n:10][cH:11][cH:12][cH:13][c:14]3[Cl:15])[cH:16][cH:17][c:18]2[c:19](=[O:20])[nH:21]1
COCC(=O)Cl.NC(=O)c1ccc(-c2ncccc2Cl)nc1N
COCc1nc2nc(-c3ncccc3Cl)ccc2c(=O)[nH]1
null
null
C1CCOC1
Aromatic Heterocycle Formation
OtherReaction
614645d801f7c5726ec106aa02b43279861de36ea60b67b39b15bd956115aa68
02d67ba88d19cec9fd983cfc9ce8356800130d81fa7c25da407b402df0800696
O=c1[nH]cnc2nc(-c3ccccn3)ccc12
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[#8:3].[NH2;D1;+0:4]-[C;H0;D3;+0:5](=[O;D1;H0:6])-[c:7](:[c:8]):[c:9](-[NH2;D1;+0:10]):[#7;a:11]:[c:12]>>[#8:3]-[C:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:10]:[c:9](:[#7;a:11]:[c:12]):[c:7](:[c:8]):[c;H0;D3;+0:5](=[O;D1;H0:6]):[nH;D2;+0:4]:1
null
[]
null
null
8
HOUR
Dissolve 6-amino-3′-chloro-[2,2′]bipyridinyl-5-carboxylic acid amide (0.5 g, 2.02 mmol) in anhydrous THF (10 mL) under N2 atmosphere. Add drop wise pyridine (0.36 g, 4.04 mmol) and methoxyacetyl chloride (0.48 g, 4.04 mmol) to the reaction mixture and stir at room temperature overnight. Add 10% aq. NaOH (10 mL) and ref...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amide.Primary amine
null
c1ccncc1
c1ccc2cncnc2n1
c1ccc2cncnc2n1.c1ccncc1
HCl
C1CCOC1
null
8
COCC(=O)Cl.NC(=O)c1ccc(-c2ncccc2Cl)nc1N>C1CCOC1>COCc1nc2nc(-c3ncccc3Cl)ccc2c(=O)[nH]1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a3cbbc97b49b4f18939c73ad6166cc7a
COCc1nc2nc(-c3ncccc3Cl)ccc2c(=O)[nH]1.O=P(Cl)(Cl)Cl>>COCc1nc(Cl)c2ccc(-c3ncccc3Cl)nc2n1
ClC=1C(=NC=CC1)C=1C=CC2=C(N=C(NC2=O)COC)N1.N1=C(C=CC=C1C)C.O=P(Cl)(Cl)Cl>>ClC=1C2=C(N=C(N1)COC)N=C(C=C2)C2=NC=CC=C2Cl
O=[c:6]1[nH:5][c:4]([CH2:3][O:2][CH3:1])[n:21][c:20]2[c:8]1[cH:9][cH:10][c:11](-[c:12]1[n:13][cH:14][cH:15][cH:16][c:17]1[Cl:18])[n:19]2.O=P(Cl)(Cl)[Cl:7]>>[CH3:1][O:2][CH2:3][c:4]1[n:5][c:6]([Cl:7])[c:8]2[cH:9][cH:10][c:11](-[c:12]3[n:13][cH:14][cH:15][cH:16][c:17]3[Cl:18])[n:19][c:20]2[n:21]1
COCc1nc2nc(-c3ncccc3Cl)ccc2c(=O)[nH]1.O=P(Cl)(Cl)Cl
COCc1nc(Cl)c2ccc(-c3ncccc3Cl)nc2n1
null
null
C(Cl)(Cl)Cl
Functional Group Interconversion
OtherReaction
d47976970a5d5230c47ef65f20d9160cb77827992ffb6b76ceab53d201153dd5
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc(-c2ccc3cncnc3n2)nc1
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].O=[c;H0;D3;+0:2]1:[nH;D2;+0:3]:[c:4](-[C:5]):[#7;a:6]:[c:7](:[#7;a:8]:[c:9]):[c:10]:1:[c:11]>>[C:5]-[c:4]1:[#7;a:6]:[c:7](:[#7;a:8]:[c:9]):[c:10](:[c:11]):[c;H0;D3;+0:2](-[Cl;H0;D1;+0:1]):[n;H0;D2;+0:3]:1
null
[]
null
null
null
null
Reflux a mixture of 7-(3-chloro-pyridin-2-yl)-2-methoxymethyl-3H-pyrido[2,3-d]pyrimidin-4-one (0.25 g), 2,6-lutidine (0.44 g), and POCl3 (0.51 g) in CHCl3 (5 mL) for 20 hours. Cool the mixture and concentrate under reduced pressure. Partition the residue between EtOAc and saturated NaHCO3 solution. Wash the EtOAc porti...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2cncnc2n1
c1cnc2ncncc2c1
c1cnc2ncncc2c1.c1ccncc1
HCl
C(Cl)(Cl)Cl
null
null
COCc1nc2nc(-c3ncccc3Cl)ccc2c(=O)[nH]1.O=P(Cl)(Cl)Cl>C(Cl)(Cl)Cl>COCc1nc(Cl)c2ccc(-c3ncccc3Cl)nc2n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a91ff830304340ea99b8ec6790e64c8a
Nc1cccc2cnccc12.O=C(Cl)C(Cl)(Cl)Cl>>O=C(Nc1cccc2cnccc12)C(Cl)(Cl)Cl
NC1=C2C=CN=CC2=CC=C1.ClC(C(=O)Cl)(Cl)Cl>>ClC(C(=O)NC1=C2C=CN=CC2=CC=C1)(Cl)Cl
[NH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12.Cl[C:2](=[O:1])[C:14]([Cl:15])([Cl:16])[Cl:17]>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12)[C:14]([Cl:15])([Cl:16])[Cl:17]
Nc1cccc2cnccc12.O=C(Cl)C(Cl)(Cl)Cl
O=C(Nc1cccc2cnccc12)C(Cl)(Cl)Cl
null
null
ClCCl.CCN(CC)CC
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc2cnccc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[Cl;D1;H0:4])(-[Cl;D1;H0:5])-[Cl;D1;H0:6].[NH2;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[Cl;D1;H0:4]-[C:3](-[Cl;D1;H0:5])(-[Cl;D1;H0:6])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10]
65.1
[{"value": 65.0, "product": "ClC(C(=O)NC1=C2C=CN=CC2=CC=C1)(Cl)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 65.1, "product": "ClC(C(=O)NC1=C2C=CN=CC2=CC=C1)(Cl)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
14
HOUR
A solution of 5-aminoisoquinoline (1.0 g, 6.9 mmol) in dichloromethane (40 mL) and Et3N (1 mL) at 5° C. was treated with trichloroacetyl chloride (1.38 g, 7.6 mmol) dropwise. The reaction mixture was stirred at ambient temperature for 14 hours, concentrated, diluted with ethyl acetate and washed with 1N HCl. The aqueou...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2cnccc2c1
HCl
ClCCl.CCN(CC)CC
null
14
Nc1cccc2cnccc12.O=C(Cl)C(Cl)(Cl)Cl>ClCCl.CCN(CC)CC>O=C(Nc1cccc2cnccc12)C(Cl)(Cl)Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-024b250d20b24d2abbbcdd14f7613d24
C1CCC2=NCCCN2CC1.CCOC(C)=O.NCCc1cccc(F)c1>>O=C(NCCc1cccc(F)c1)Nc1cccc2cnccc12
C(C)(=O)OCC.C1CCC2=NCCCN2CC1.FC=1C=C(C=CC1)CCN>>FC=1C=C(C=CC1)CCNC(=O)NC1=C2C=CN=CC2=CC=C1
[N:13]1=[C:18]2[N:20]([CH2:19][CH2:16][CH2:17][CH2:22][CH2:23]2)[CH2:21][CH2:15][CH2:14]1.CCO[C:2](C)=[O:1].[NH2:3][CH2:4][CH2:5][c:6]1[cH:7][cH:8][cH:9][c:10]([F:11])[cH:12]1>>[O:1]=[C:2]([NH:3][CH2:4][CH2:5][c:6]1[cH:7][cH:8][cH:9][c:10]([F:11])[cH:12]1)[NH:13][c:14]1[cH:15][cH:16][cH:17][c:18]2[cH:19][n:20][cH:21][c...
C1CCC2=NCCCN2CC1.CCOC(C)=O.NCCc1cccc(F)c1
O=C(NCCc1cccc(F)c1)Nc1cccc2cnccc12
null
null
C(C)#N
Aromatic Heterocycle Formation
OtherReaction
3611f44769d386b1bfe0c5b8c8d1388cb7f87a5a7a8498354be7aa1dd3b6c426
1da510b4e3613d637593754dc05473127c6553dbe8838e5750afa76b7abe6f45
O=C(NCCc1ccccc1)Nc1cccc2cnccc12
C-C-O-[C;H0;D3;+0:1](-C)=[O;D1;H0:2].[CH2;D2;+0:3]1-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[N;H0;D3;+0:6]2-[CH2;D2;+0:7]-[CH2;D2;+0:8]-[CH2;D2;+0:9]-[CH2;D2;+0:10]-[CH2;D2;+0:11]-[C;H0;D3;+0:12]-2=[N;H0;D2;+0:13]-1.[C:14]-[C:15]-[NH2;D1;+0:16]>>[C:14]-[C:15]-[NH;D2;+0:16]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:13]-[c;H0;D3;+0:3]1...
65
[{"value": 65.0, "product": "FC=1C=C(C=CC1)CCNC(=O)NC1=C2C=CN=CC2=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The product from Example 1A (0.65 g, 2.25 mmol), DBU (0.85 g, 5.6 mmol) and 2-(3-fluorophenyl)ethylamine (0.35 g, 2.5 mmol) in acetonitrile (50 mL) were refluxed for 10 hours. The mixture was cooled, concentrated, diluted with ethyl acetate, washed twice with aqueous ammonium chloride and concentrated to dryness. The s...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine.Tertiary amine
Urea
C1CCC2=NCCCN2CC1
c1ccc2cnccc2c1
c1ccccc1.c1ccc2cnccc2c1
HO-
C(C)#N
null
null
C1CCC2=NCCCN2CC1.CCOC(C)=O.NCCc1cccc(F)c1>C(C)#N>O=C(NCCc1cccc(F)c1)Nc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-53554113e33343818790da31833728e8
Cc1cc2c(N)cccc2nn1.O=C(Cl)C(Cl)(Cl)Cl>>Cc1cc2c(NC(=O)C(Cl)(Cl)Cl)cccc2nn1
CC=1N=NC=2C=CC=C(C2C1)N.ClC(C(=O)Cl)(Cl)Cl>>ClC(C(=O)NC1=C2C=C(N=NC2=CC=C1)C)(Cl)Cl
[CH3:1][c:2]1[cH:3][c:4]2[c:5]([NH2:6])[cH:13][cH:14][cH:15][c:16]2[n:17][n:18]1.Cl[C:7](=[O:8])[C:9]([Cl:10])([Cl:11])[Cl:12]>>[CH3:1][c:2]1[cH:3][c:4]2[c:5]([NH:6][C:7](=[O:8])[C:9]([Cl:10])([Cl:11])[Cl:12])[cH:13][cH:14][cH:15][c:16]2[n:17][n:18]1
Cc1cc2c(N)cccc2nn1.O=C(Cl)C(Cl)(Cl)Cl
Cc1cc2c(NC(=O)C(Cl)(Cl)Cl)cccc2nn1
null
null
C(C)N(CC)CC
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc2nnccc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[Cl;D1;H0:4])(-[Cl;D1;H0:5])-[Cl;D1;H0:6].[#7;a:7]:[c:8]:[c:9]:[c:10](-[NH2;D1;+0:11]):[c:12]>>[#7;a:7]:[c:8]:[c:9]:[c:10](-[NH;D2;+0:11]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[Cl;D1;H0:4])(-[Cl;D1;H0:5])-[Cl;D1;H0:6]):[c:12]
null
[]
null
null
null
null
The title compound was prepared using 3-methylcinnolin-5-amine (commercially available Maybridge), triethylamine, trichloroacetyl chloride and the procedure described in Example 1A. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2nnccc2c1
HCl
C(C)N(CC)CC
null
null
Cc1cc2c(N)cccc2nn1.O=C(Cl)C(Cl)(Cl)Cl>C(C)N(CC)CC>Cc1cc2c(NC(=O)C(Cl)(Cl)Cl)cccc2nn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dd3cfb7d3b544124813d63fb69494554
Cc1cc2c(NC(=O)C(Cl)(Cl)Cl)cccc2nn1.NCc1ccc(Cl)c(Cl)c1>>Cc1cc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc2nn1
ClC=1C=C(CN)C=CC1Cl.ClC(C(=O)NC1=C2C=C(N=NC2=CC=C1)C)(Cl)Cl.C1CCC2=NCCCN2CC1>>ClC=1C=C(CNC(=O)NC2=C3C=C(N=NC3=CC=C2)C)C=CC1Cl
ClC(Cl)(Cl)[C:7]([NH:6][c:5]1[c:4]2[cH:3][c:2]([CH3:1])[n:24][n:23][c:22]2[cH:21][cH:20][cH:19]1)=[O:8].[NH2:9][CH2:10][c:11]1[cH:12][cH:13][c:14]([Cl:15])[c:16]([Cl:17])[cH:18]1>>[CH3:1][c:2]1[cH:3][c:4]2[c:5]([NH:6][C:7](=[O:8])[NH:9][CH2:10][c:11]3[cH:12][cH:13][c:14]([Cl:15])[c:16]([Cl:17])[cH:18]3)[cH:19][cH:20][c...
Cc1cc2c(NC(=O)C(Cl)(Cl)Cl)cccc2nn1.NCc1ccc(Cl)c(Cl)c1
Cc1cc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc2nn1
null
null
null
Acylation
OtherReaction
ffe5fdd6070c0c75bd20e0ee13bc090c32d3281269178f04f3649ea77b9456e8
56b69d37f244d2e25fa681709adac1c85312cc9ccbfef016678a99d56e55b4c6
O=C(NCc1ccccc1)Nc1cccc2nnccc12
Cl-C(-Cl)(-Cl)-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3]-[c:4].[NH2;D1;+0:5]-[C:6]-[c:7]>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[#7:3]-[c:4])-[NH;D2;+0:5]-[C:6]-[c:7]
null
[]
null
null
null
null
The title compound was prepared using 3,4-dichlorobenzylamine, the product from Example 16A, DBU and the procedure described in Example 1B. MS (ESI+) m/z 362 (M+)+; 1H NMR (DMSO-d6) δ 2.88 (s, 3H), 4.36 (d, 2H), 7.10 (t, 1H), 7.34 (dd, 1H), 7.59 (m, 2H), 7.76 (t, 1H), 8.04 (d, 2H), 8.19 (d, 1H), 8.93 (s, 1H). Condition...
10.6084/m9.figshare.5104873.v1
null
Trichloro group.Secondary amide.Primary amine
Urea
null
null
c1ccccc1.c1ccc2nnccc2c1
HCl
null
null
null
Cc1cc2c(NC(=O)C(Cl)(Cl)Cl)cccc2nn1.NCc1ccc(Cl)c(Cl)c1>>Cc1cc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc2nn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-264a7560bdc047b6b11ed3aa62c5ca72
O=C1CCC(=O)N1Br.c1ccc2cnccc2c1>>Brc1cccc2cnccc12
C1=NC=CC2=CC=CC=C12.OS(=O)(=O)O.[NH4+].[OH-].BrN1C(CCC1=O)=O>>BrC1=C2C=CN=CC2=CC=C1
O=C1CCC(=O)N1[Br:1].[cH:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][n:8][cH:9][cH:10][c:11]12>>[Br:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][n:8][cH:9][cH:10][c:11]12
O=C1CCC(=O)N1Br.c1ccc2cnccc2c1
Brc1cccc2cnccc12
null
null
CCCCCCC
Functional Group Interconversion
Bromination
9cac9f3adaa01c5b3ba77ecc78b3325ca368823796a491b3ff1d81b1acdc724d
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccc2cnccc2c1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[c:2]:[c:3]:[cH;D2;+0:4]:[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:4](:[c:3]:[c:2]):[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1
null
[]
-10
CELSIUS
null
null
Concentrated H2SO4 (260 mL) was cooled to −25° C. while stirring with a mechanical stirrer. Isoquinoline (30 mL, 0.25 mol) was added slowly so the temperature did not exceed 0° C. After the addition was complete, the red solution was recooled to −25° C. and treated with N-bromosuccinimide (55.49 g, 0.31 mol) in small p...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
C1CCNC1.c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HO-
CCCCCCC
-10
null
O=C1CCC(=O)N1Br.c1ccc2cnccc2c1>CCCCCCC>Brc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e82ad2e910d1448f86a850a6cac03894
Brc1cccc2cnccc12>>O=[N+]([O-])c1ccc(Br)c2ccncc12
BrC1=C2C=CN=CC2=CC=C1.[N+](=O)([O-])[O-].[K+]>>BrC1=C2C=CN=CC2=C(C=C1)[N+](=O)[O-]
[cH:4]1[cH:5][cH:6][c:7]([Br:8])[c:9]2[cH:10][cH:11][n:12][cH:13][c:14]12>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([Br:8])[c:9]2[cH:10][cH:11][n:12][cH:13][c:14]12
Brc1cccc2cnccc12
O=[N+]([O-])c1ccc(Br)c2ccncc12
null
null
[OH-].[NH4+]
Functional Group Addition
OtherReaction
af041d80e34a3ce46b5eb910f230615587e5ab9eb4305ac845f1ae2dbd577a25
22f3183026a2d99c91ec0c53f0059a15c8421016bd62c8ab45281362b96dc686
c1ccc2cnccc2c1
[c:1]:[#7;a:2]:[c:3]:[c:4](:[c:5]):[cH;D2;+0:6]:[c:7]:[c:8]>>[O;-;D1;H0:9]-[#7;+:10](=[O;D1;H0:11])-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:4](:[c:5]):[c:3]:[#7;a:2]:[c:1]
null
[]
null
null
1
HOUR
The diethyl ether solution from Example 57A was treated with potassium nitrate (10.1 g, 100 mmol). After stirring for one hour, The mixture was poured onto ice and neutralized with concentrated ammonium hydroxide (˜300 ml). The crude product was collected by filtration, dried, and recrystalization from methanol to prov...
10.6084/m9.figshare.5104873.v1
null
null
Nitro group
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
Other
[OH-].[NH4+]
null
1
Brc1cccc2cnccc12>[OH-].[NH4+]>O=[N+]([O-])c1ccc(Br)c2ccncc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cdbc8cf33a7841f9b75f923182e141ef
O=[N+]([O-])c1ccc(Br)c2ccncc12>>Nc1cccc2ccncc12
BrC1=C2C=CN=CC2=C(C=C1)[N+](=O)[O-]>>C1=NC=CC2=CC=CC(=C12)N
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][c:5](Br)[c:6]2[cH:7][cH:8][n:9][cH:10][c:11]12>>[NH2:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][cH:8][n:9][cH:10][c:11]12
O=[N+]([O-])c1ccc(Br)c2ccncc12
Nc1cccc2ccncc12
null
[Pd]
null
Reduction
OtherReaction
33243a7a0a86654ba62ab63c9b0595dc06b3b2ec6c8d660470131d23402a9f9a
7a1074c91f17781b9c7c26911e795314b42511dc69433b1dc4bc93ccba503456
c1ccc2cnccc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](-[N+;H0;D3:5](=O)-[O-]):[c:6]2:[c:7]:[#7;a:8]:[c:9]:[c:10]:[c:11]:2:1>>[NH2;D1;+0:5]-[c:4]1:[c:3]:[c:2]:[cH;D2;+0:1]:[c:11]2:[c:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:1:2
null
[]
null
null
null
null
The product from Example 57B was treated with Pd/C under a hydrogen atmosphere to provide the title compound. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Nitro group
Primary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
Br-
[Pd]
null
null
O=[N+]([O-])c1ccc(Br)c2ccncc12>[Pd]>Nc1cccc2ccncc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b30b419672b0479ba052baffaacb2fbf
Nc1cccc2ccncc12.O=C(Cl)C(Cl)(Cl)Cl>>O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl
C1=NC=CC2=CC=CC(=C12)N.ClC(C(=O)Cl)(Cl)Cl>>ClC(C(=O)NC=1C=CC=C2C=CN=CC12)(Cl)Cl
[NH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][cH:10][n:11][cH:12][c:13]12.Cl[C:2](=[O:1])[C:14]([Cl:15])([Cl:16])[Cl:17]>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][cH:10][n:11][cH:12][c:13]12)[C:14]([Cl:15])([Cl:16])[Cl:17]
Nc1cccc2ccncc12.O=C(Cl)C(Cl)(Cl)Cl
O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl
null
null
null
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc2cnccc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[Cl;D1;H0:4])(-[Cl;D1;H0:5])-[Cl;D1;H0:6].[#7;a:7]:[c:8]:[c:9]:[c:10](-[NH2;D1;+0:11]):[c:12]>>[#7;a:7]:[c:8]:[c:9]:[c:10](-[NH;D2;+0:11]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[Cl;D1;H0:4])(-[Cl;D1;H0:5])-[Cl;D1;H0:6]):[c:12]
null
[]
null
null
null
null
The product from Example 57C and trichloroacetylchloride were processed as described in Example 1A to provide the title compound. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2cnccc2c1
HCl
null
null
null
Nc1cccc2ccncc12.O=C(Cl)C(Cl)(Cl)Cl>>O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c9ac0b31af9b424dafeeed6462c070b2
NCc1ccc(C(F)(F)F)cc1.O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl>>O=C(NCc1ccc(C(F)(F)F)cc1)Nc1cccc2ccncc12
FC(C1=CC=C(CN)C=C1)(F)F.ClC(C(=O)NC=1C=CC=C2C=CN=CC12)(Cl)Cl.C1CCC2=NCCCN2CC1>>C1=NC=CC2=CC=CC(=C12)NC(=O)NCC1=CC=C(C=C1)C(F)(F)F
[NH2:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[cH:13][cH:14]1.ClC(Cl)(Cl)[C:2](=[O:1])[NH:15][c:16]1[cH:17][cH:18][cH:19][c:20]2[cH:21][cH:22][n:23][cH:24][c:25]12>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[cH:13][cH:14]1)[NH:15][c:16]1[cH:17][cH:18][cH:19][c:20]2...
NCc1ccc(C(F)(F)F)cc1.O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl
O=C(NCc1ccc(C(F)(F)F)cc1)Nc1cccc2ccncc12
null
null
null
Acylation
OtherReaction
ffe5fdd6070c0c75bd20e0ee13bc090c32d3281269178f04f3649ea77b9456e8
56b69d37f244d2e25fa681709adac1c85312cc9ccbfef016678a99d56e55b4c6
O=C(NCc1ccccc1)Nc1cccc2ccncc12
Cl-C(-Cl)(-Cl)-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3]-[c:4].[NH2;D1;+0:5]-[C:6]-[c:7]>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[#7:3]-[c:4])-[NH;D2;+0:5]-[C:6]-[c:7]
null
[]
null
null
null
null
The title compound was prepared using 4-(trifluoromethyl)benzylamine, the product from Example 57D, DBU and the procedure described in Example 1B. MS (ESI+) m/z 346 (M+H)+; 1H NMR (DMSO-d6) δ 9.58 (s, 1H), 9.10 (s, 1H), 8.49 (d, 1H), 8.12 (d, 1H), 7.81-7.54 (m, 7H), 7.20 (t, 1H), 4.47 (d, 2H); Anal. Calcd for C18H14F3N...
10.6084/m9.figshare.5104873.v1
null
Trichloro group.Secondary amide.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
HCl
null
null
null
NCc1ccc(C(F)(F)F)cc1.O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl>>O=C(NCc1ccc(C(F)(F)F)cc1)Nc1cccc2ccncc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f92abbcdc3c94b179fa768fab3bf8f4d
NCc1ccc(Br)cc1.O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl>>O=C(NCc1ccc(Br)cc1)Nc1cccc2ccncc12
O.BrC1=CC=C(CN)C=C1.ClC(C(=O)NC=1C=CC=C2C=CN=CC12)(Cl)Cl.C1CCC2=NCCCN2CC1>>BrC1=CC=C(CNC(=O)NC=2C=CC=C3C=CN=CC23)C=C1
[NH2:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Br:9])[cH:10][cH:11]1.ClC(Cl)(Cl)[C:2](=[O:1])[NH:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[cH:18][cH:19][n:20][cH:21][c:22]12>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Br:9])[cH:10][cH:11]1)[NH:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[cH:18][cH:19][n:20][cH:21][c:22]12
NCc1ccc(Br)cc1.O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl
O=C(NCc1ccc(Br)cc1)Nc1cccc2ccncc12
null
null
CO
Acylation
OtherReaction
ffe5fdd6070c0c75bd20e0ee13bc090c32d3281269178f04f3649ea77b9456e8
56b69d37f244d2e25fa681709adac1c85312cc9ccbfef016678a99d56e55b4c6
O=C(NCc1ccccc1)Nc1cccc2ccncc12
Cl-C(-Cl)(-Cl)-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3]-[c:4].[NH2;D1;+0:5]-[C:6]-[c:7]>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[#7:3]-[c:4])-[NH;D2;+0:5]-[C:6]-[c:7]
null
[]
null
null
null
null
The title compound was prepared using 4-bromobenzylamine, the product from Example 57D, DBU and the procedure described in Example 1B. MS (ESI+) m/z 356 (M+H)+; 1H NMR (DMSO-d6) δ 9.52 (s, 1H), 9.15 (s, 1H), 8.49 (d, 1H), 8.11 (d, 1H), 7.77 (d, 1H), 7.67 (t, 1H), 7.55 (m, 3H) 7.32 (d, 2H), 7.25 (t, 1H), 4.34 (d, 2H); A...
10.6084/m9.figshare.5104873.v1
null
Trichloro group.Secondary amide.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
HCl
CO
null
null
NCc1ccc(Br)cc1.O=C(Nc1cccc2ccncc12)C(Cl)(Cl)Cl>CO>O=C(NCc1ccc(Br)cc1)Nc1cccc2ccncc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ac589d79f7aa450e9af1dc8575d8944e
O=C(O)Cc1ccccc1C(=O)O.[NH4+]>>O=C1Cc2ccccc2C(=O)N1
C(=O)(O)CC1=C(C(=O)O)C=CC=C1.[NH4+].[OH-]>>C1(NC(CC2=CC=CC=C12)=O)=O
O[C:2](=[O:1])[CH2:3][c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[C:10](O)=[O:11].[NH4+:12]>>[O:1]=[C:2]1[CH2:3][c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[C:10](=[O:11])[NH:12]1
O=C(O)Cc1ccccc1C(=O)O.[NH4+]
O=C1Cc2ccccc2C(=O)N1
null
null
null
Acylation
OtherReaction
8c6e19b6d9556b641f610ee6f3892dfc89bcb6dcf68cea638ca6db03bf9c2edb
286fbd2cccb868855ca34a2d629ab8d8113cbdbf5f1fb5f1c2174808f1aa7a3a
O=C1Cc2ccccc2C(=O)N1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]-[C:6]-[C;H0;D3;+0:7](-O)=[O;D1;H0:8].[NH4+;D0:9]>>[O;D1;H0:2]=[C;H0;D3;+0:1]1-[NH;D2;+0:9]-[C;H0;D3;+0:7](=[O;D1;H0:8])-[C:6]-[c:5]:[c:3]-1:[c:4]
74
[{"value": 74.0, "product": "C1(NC(CC2=CC=CC=C12)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
200
CELSIUS
8
HOUR
2-(Carboxymethyl)benzoic acid (10 g, 55.6 mmol) was dissolved in concentrated NH4OH (15 mL) and then was evaporated to dryness under reduced pressure. The process was repeated with additional NH4OH (5 mL). The resulting residue was treated with 1,2-dichlorobenzene (20 mL) and heated with stirring at 200° C. without a c...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Carboxylic acid
Unsubstituted dicarboximide
null
c1ccc2c(c1)CCNC2
c1ccc2c(c1)CCNC2
HO-
null
200
8
O=C(O)Cc1ccccc1C(=O)O.[NH4+]>>O=C1Cc2ccccc2C(=O)N1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cc77105416774ff4acba9c435d4af89e
Clc1cc2ccccc2c(Cl)n1>>Clc1cc2ccccc2cn1
ClC1=NC(=CC2=CC=CC=C12)Cl.Cl.[Sn]>>ClC=1N=CC2=CC=CC=C2C1
Cl[c:10]1[c:9]2[c:4]([cH:3][c:2]([Cl:1])[n:11]1)[cH:5][cH:6][cH:7][cH:8]2>>[Cl:1][c:2]1[cH:3][c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[cH:10][n:11]1
Clc1cc2ccccc2c(Cl)n1
Clc1cc2ccccc2cn1
null
null
C(C)(=O)O
Functional Group Interconversion
Aromatic dehalogenation
5f52289b2baf4c41a4fd744ce2a94a34156399db711c7ce043a5818b3fd25f7a
56de34d4a44cb25d9380269ee5e138b0f24b40a3a0db22c5508049dc775a861f
c1ccc2cnccc2c1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](:[c:5]):[c:6]>>[c:3]:[#7;a:2]:[cH;D2;+0:1]:[c:4](:[c:5]):[c:6]
23
[{"value": 23.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
57.5
CELSIUS
null
null
The product from Example 60B (6.73 g, 33.8 mmol) was suspended in glacial acetic acid (37 mL) and concentrated HCl (13 mL), treated with tin powder (12.1 g, 101.9 mmol), and heated at 55-60° C. for 3 hours with stirring. The mixture was allowed to cool to room temperature and the precipitated tin salts were removed by ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
Other
C(C)(=O)O
57.5
null
Clc1cc2ccccc2c(Cl)n1>C(C)(=O)O>Clc1cc2ccccc2cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d5ccbe39f41541a1a5bf6cc3514f6406
Nc1cccc2cnccc12.O=C(Cl)Cl>>O=C=Nc1cccc2cnccc12
C(=O)(Cl)Cl.NC1=C2C=CN=CC2=CC=C1>>N(=C=O)C1=C2C=CN=CC2=CC=C1
[NH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12.Cl[C:2](Cl)=[O:1]>>[O:1]=[C:2]=[N:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12
Nc1cccc2cnccc12.O=C(Cl)Cl
O=C=Nc1cccc2cnccc12
null
CN(C)C=1C=CN=CC1
C(Cl)Cl
Miscellaneous
OtherReaction
7d3fae5ca5d4875eff5b8b9cc12bb45e992207dcc8962ac035cf5aaf63f27286
5e78fe62a292da2c55590df217f7e190c26df27095ff0827e6cc86b7659890bd
c1ccc2cnccc2c1
Cl-[C;H0;D3;+0:1](-Cl)=[O;D1;H0:2].[NH2;D1;+0:3]-[c:4](:[c:5]):[c:6]>>[O;D1;H0:2]=[C;H0;D2;+0:1]=[N;H0;D2;+0:3]-[c:4](:[c:5]):[c:6]
null
[]
null
null
8
HOUR
Phosgene (20 ml, 20% in toluene from Fluka) in CH2Cl2 (300 mL) at 0° C. was treated with DMAP (10 g) in CH2Cl2 (100 mL) slowly. After complete addition, the mixture was treated with 5-aminoisoquinoline (5 g) in CH2Cl2 (100 mL) dropwise. The mixture was allowed to warm to room temperature and then stirred overnight. The...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Primary amine
Isocyanate
null
null
c1ccc2cnccc2c1
HCl
CN(C)C=1C=CN=CC1.C(Cl)Cl
null
8
Nc1cccc2cnccc12.O=C(Cl)Cl>CN(C)C=1C=CN=CC1.C(Cl)Cl>O=C=Nc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a014e40984194ad18ac351616be7b53c
N#Cc1ccc(CO)cc1.O=C=Nc1cccc2cnccc12>>N#Cc1ccc(COC(=O)Nc2cccc3cnccc23)cc1
C(#N)C1=CC=C(CO)C=C1.N(=C=O)C1=C2C=CN=CC2=CC=C1>>C1=NC=CC2=C(C=CC=C12)NC(OCC1=CC=C(C=C1)C#N)=O
[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][OH:8])[cH:22][cH:23]1.[C:9](=[O:10])=[N:11][c:12]1[cH:13][cH:14][cH:15][c:16]2[cH:17][n:18][cH:19][cH:20][c:21]12>>[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][O:8][C:9](=[O:10])[NH:11][c:12]2[cH:13][cH:14][cH:15][c:16]3[cH:17][n:18][cH:19][cH:20][c:21]23)[cH:22][cH:23]1
N#Cc1ccc(CO)cc1.O=C=Nc1cccc2cnccc12
N#Cc1ccc(COC(=O)Nc2cccc3cnccc23)cc1
null
null
null
Protection
OtherReaction
8d2aa5da7fec498749aba98cc9467e8d82c146f343570568bec74a92b10e0ae2
e505c5de73b3f9ad0414c141c59109424d376f26a728bbd154d3edfd03d2f50a
O=C(Nc1cccc2cnccc12)OCc1ccccc1
[O;D1;H0:1]=[C;H0;D2;+0:2]=[N;H0;D2;+0:3]-[c:4](:[c:5]):[c:6].[OH;D1;+0:7]-[C:8]-[c:9]>>[O;D1;H0:1]=[C;H0;D3;+0:2](-[NH;D2;+0:3]-[c:4](:[c:5]):[c:6])-[O;H0;D2;+0:7]-[C:8]-[c:9]
44
[{"value": 44.0, "product": "C1=NC=CC2=C(C=CC=C12)NC(OCC1=CC=C(C=C1)C#N)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
4-Cyanobenzyl alcohol (150 mg, 1.13 mmol) diethyl ether (10 mL) was treated with the product from Example 61A as an ethereal solution. The mixture was stirred for 2 hours, filtered, and the filter cake was washed with diethyl ether to provide the title compound as an off-white solid (150 mg, 44%). 1H HMR (300 MHz, DMSO...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary alcohol
Carbamic ester
null
null
c1ccccc1.c1ccc2cnccc2c1
null
null
null
2
N#Cc1ccc(CO)cc1.O=C=Nc1cccc2cnccc12>>N#Cc1ccc(COC(=O)Nc2cccc3cnccc23)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-896af839f2e74d45a7df1a4bdd6efa4e
Cc1cc2c(N)cccc2cn1.O=C=NCc1ccc(Br)cc1>>Cc1cc2c(NC(=O)NCc3ccc(Br)cc3)cccc2cn1
CC=1N=CC=2C=CC=C(C2C1)N.BrC1=CC=C(C=C1)CN=C=O>>BrC1=CC=C(C=C1)CNC(=O)NC1=C2C=C(N=CC2=CC=C1)C
[CH3:1][c:2]1[cH:3][c:4]2[c:5]([NH2:6])[cH:18][cH:19][cH:20][c:21]2[cH:22][n:23]1.[C:7](=[O:8])=[N:9][CH2:10][c:11]1[cH:12][cH:13][c:14]([Br:15])[cH:16][cH:17]1>>[CH3:1][c:2]1[cH:3][c:4]2[c:5]([NH:6][C:7](=[O:8])[NH:9][CH2:10][c:11]3[cH:12][cH:13][c:14]([Br:15])[cH:16][cH:17]3)[cH:18][cH:19][cH:20][c:21]2[cH:22][n:23]1
Cc1cc2c(N)cccc2cn1.O=C=NCc1ccc(Br)cc1
Cc1cc2c(NC(=O)NCc3ccc(Br)cc3)cccc2cn1
null
null
C1(=CC=CC=C1)C
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[NH;D2;+0:7]-[C:8]-[c:9]
null
[]
80
CELSIUS
null
null
The product from Example 63A (500 mg, 3.1 mmol) in toluene (10 mL) was treated with 1-bromo-4-(isocyanatomethyl)benzene (0.5 mL, 3.57 mmol) with stirring and then the mixture was heated at 80° C. overnight. The mixture was allowed to cool to room temperature, filtered, the filter cake was washed with toluene, and allow...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
C1(=CC=CC=C1)C
80
null
Cc1cc2c(N)cccc2cn1.O=C=NCc1ccc(Br)cc1>C1(=CC=CC=C1)C>Cc1cc2c(NC(=O)NCc3ccc(Br)cc3)cccc2cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-09aa8922b041445ba2af6c40b03ec737
Nc1cccc2c(Cl)nccc12.O=C=NCc1ccc(Br)cc1>>O=C(NCc1ccc(Br)cc1)Nc1cccc2c(Cl)nccc12
ClC1=NC=CC=2C(=CC=CC12)N.BrC1=CC=C(C=C1)CN=C=O>>BrC1=CC=C(C=C1)CNC(=O)NC1=C2C=CN=C(C2=CC=C1)Cl
[NH2:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[c:18]([Cl:19])[n:20][cH:21][cH:22][c:23]12.[O:1]=[C:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Br:9])[cH:10][cH:11]1>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Br:9])[cH:10][cH:11]1)[NH:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[c:18]([Cl:19])[n:20][cH:21][cH:22][c:23]12
Nc1cccc2c(Cl)nccc12.O=C=NCc1ccc(Br)cc1
O=C(NCc1ccc(Br)cc1)Nc1cccc2c(Cl)nccc12
null
null
C1(=CC=CC=C1)C
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[NH;D2;+0:7]-[C:8]-[c:9]
63.1
[{"value": 63.0, "product": "BrC1=CC=C(C=C1)CNC(=O)NC1=C2C=CN=C(C2=CC=C1)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 63.1, "product": "BrC1=CC=C(C=C1)CNC(=O)NC1=C2C=CN=C(C2=CC=C1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
90
CELSIUS
null
null
The product from Example 64A (520 mg, 2.91 mmol) in toluene (8 mL) was treated with 1-bromo-4-(isocyanatomethyl)benzene (0.41 mL, 2.93 mmol) with stirring and then the mixture was heated at 90° C. for 2 hours. The mixture was allowed to cool to room temperature, filtered, the filter cake washed with toluene, and air-dr...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
C1(=CC=CC=C1)C
90
null
Nc1cccc2c(Cl)nccc12.O=C=NCc1ccc(Br)cc1>C1(=CC=CC=C1)C>O=C(NCc1ccc(Br)cc1)Nc1cccc2c(Cl)nccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-53af5ae1b742411193551ab8a30ba92a
Cc1nccc2c(N)cccc12.O=C=NCc1ccc(Br)cc1>>Cc1nccc2c(NC(=O)NCc3ccc(Br)cc3)cccc12
CC1=NC=CC=2C(=CC=CC12)N.BrC1=CC=C(C=C1)CN=C=O>>BrC1=CC=C(C=C1)CNC(=O)NC1=C2C=CN=C(C2=CC=C1)C
[CH3:1][c:2]1[n:3][cH:4][cH:5][c:6]2[c:7]([NH2:8])[cH:20][cH:21][cH:22][c:23]12.[C:9](=[O:10])=[N:11][CH2:12][c:13]1[cH:14][cH:15][c:16]([Br:17])[cH:18][cH:19]1>>[CH3:1][c:2]1[n:3][cH:4][cH:5][c:6]2[c:7]([NH:8][C:9](=[O:10])[NH:11][CH2:12][c:13]3[cH:14][cH:15][c:16]([Br:17])[cH:18][cH:19]3)[cH:20][cH:21][cH:22][c:23]12
Cc1nccc2c(N)cccc12.O=C=NCc1ccc(Br)cc1
Cc1nccc2c(NC(=O)NCc3ccc(Br)cc3)cccc12
null
null
C1(=CC=CC=C1)C
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:7]-[C:8]-[c:9])-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
90
CELSIUS
null
null
The product from Example 65A (480 mg, 3.04 mmol) in toluene (9 mL) was treated with 1-bromo-4-(isocyanatomethyl)benzene (0.43, 3.07 mmol) with stirring. After heating the mixture at 90° C. for 1 hour, the mixture was allowed to cool to room temperature, filtered, and the filter cake washed with toluene to provide the t...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
C1(=CC=CC=C1)C
90
null
Cc1nccc2c(N)cccc12.O=C=NCc1ccc(Br)cc1>C1(=CC=CC=C1)C>Cc1nccc2c(NC(=O)NCc3ccc(Br)cc3)cccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d8ab7911edad41d98ae14adb182cb303
C1COCCN1.N#Cc1ccc(F)cc1>>N#Cc1ccc(N2CCOCC2)cc1
FC1=CC=C(C#N)C=C1.N1CCOCC1.O>>N1(CCOCC1)C1=CC=C(C#N)C=C1
[NH:7]1[CH2:8][CH2:9][O:10][CH2:11][CH2:12]1.F[c:6]1[cH:5][cH:4][c:3]([C:2]#[N:1])[cH:14][cH:13]1>>[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([N:7]2[CH2:8][CH2:9][O:10][CH2:11][CH2:12]2)[cH:13][cH:14]1
C1COCCN1.N#Cc1ccc(F)cc1
N#Cc1ccc(N2CCOCC2)cc1
null
null
CS(=O)C
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation secondary amine
a47b7d43ef99c1989f39629bd45f903079b03ac5a9d702fdbffdae93a63a79cd
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc(N2CCOCC2)cc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[#8:6]1-[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]-1>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:9]1-[C:8]-[C:7]-[#8:6]-[C:11]-[C:10]-1):[c:4]:[c:5]
80
[{"value": 80.0, "product": "N1(CCOCC1)C1=CC=C(C#N)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.8, "product": "N1(CCOCC1)C1=CC=C(C#N)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
4-Fluorobenzonitrile (1 g, 8.26 mmol) and morpholine (2.2 mL, 25.2 mmol) were combined in DMSO (25 mL) and heated at 100° C. for 2.5 hours. The mixture was allowed to cool to room temperature, poured into water, and extracted with diethyl ether. The organic extracts were combined, washed with water and brine, dried ove...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1COCCN1.c1ccccc1
c1ccccc1.C1COCC[NH]1
c1ccccc1.C1COCC[NH]1
HF
CS(=O)C
100
null
C1COCCN1.N#Cc1ccc(F)cc1>CS(=O)C>N#Cc1ccc(N2CCOCC2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-52820bdcd91c4280adbd2ff3d769d0df
N#Cc1ccc(N2CCOCC2)cc1>>NCc1ccc(N2CCOCC2)cc1
O.[OH-].[Na+].N1(CCOCC1)C1=CC=C(C#N)C=C1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>>N1(CCOCC1)C1=CC=C(C=C1)CN
[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([N:7]2[CH2:8][CH2:9][O:10][CH2:11][CH2:12]2)[cH:13][cH:14]1>>[NH2:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([N:7]2[CH2:8][CH2:9][O:10][CH2:11][CH2:12]2)[cH:13][cH:14]1
N#Cc1ccc(N2CCOCC2)cc1
NCc1ccc(N2CCOCC2)cc1
null
null
C1CCOC1
Reduction
Reduction of nitrile to amine
65bec2d9f430701d30dc9fcbe1c5418f3dfa174d67be035c50edfc71895dc9c7
e8d1bc928b94bd4f5bf4b23363ce8f88b1ce7d146ba93829e7b8ad8dbe0007a7
c1ccc(N2CCOCC2)cc1
[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[NH2;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]
23
[{"value": 23.0, "product": "N1(CCOCC1)C1=CC=C(C=C1)CN", "details": "PERCENTYIELD", "is_desired": false}, {"value": 22.5, "product": "N1(CCOCC1)C1=CC=C(C=C1)CN", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The product from Example 66A (1.24 g, 6.6 mmol) in THF (25 mL) was treated with LiAlH4 (2.5 g, 65.9 mmol) at 0° C. The mixture was allowed to warm to room temperature and then refluxed for 1 hour. The mixture was allowed to cool to room temperature and then treated with 1N NaOH carefully followed by water. The mixture ...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
c1ccccc1.C1COCC[NH]1
null
C1CCOC1
null
null
N#Cc1ccc(N2CCOCC2)cc1>C1CCOC1>NCc1ccc(N2CCOCC2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-efd459b996964986839ace8df6a1ab67
NCc1ccc(N2CCOCC2)cc1.O=C=Nc1cccc2cnccc12>>O=C(NCc1ccc(N2CCOCC2)cc1)Nc1cccc2cnccc12
N1(CCOCC1)C1=CC=C(C=C1)CN.N(=C=O)C1=C2C=CN=CC2=CC=C1>>C1=NC=CC2=C(C=CC=C12)NC(=O)NCC1=CC=C(C=C1)N1CCOCC1
[NH2:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([N:9]2[CH2:10][CH2:11][O:12][CH2:13][CH2:14]2)[cH:15][cH:16]1.[O:1]=[C:2]=[N:17][c:18]1[cH:19][cH:20][cH:21][c:22]2[cH:23][n:24][cH:25][cH:26][c:27]12>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([N:9]2[CH2:10][CH2:11][O:12][CH2:13][CH2:14]2)[cH:15][cH:16]1)[NH:17][c:18]1[cH:1...
NCc1ccc(N2CCOCC2)cc1.O=C=Nc1cccc2cnccc12
O=C(NCc1ccc(N2CCOCC2)cc1)Nc1cccc2cnccc12
null
null
C(C)OCC
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccc(N2CCOCC2)cc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[C:2]-[c:3].[O;D1;H0:4]=[C;H0;D2;+0:5]=[N;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[O;D1;H0:4]=[C;H0;D3;+0:5](-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9])-[NH;D2;+0:1]-[C:2]-[c:3]
null
[]
null
null
null
null
The product from Example 66B (285 mg, 1.48 mmol) in diethyl ether (10 mL) was treated with the product from Example 61A. The mixture was filtered and the filter cake purified by chromatography (95:5 CH2Cl2—MeOH, eluant) to provide that title compound as a white solid. The corresponding di-hydrochloride salt was prepare...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.C1COCC[NH]1.c1ccc2cnccc2c1
null
C(C)OCC
null
null
NCc1ccc(N2CCOCC2)cc1.O=C=Nc1cccc2cnccc12>C(C)OCC>O=C(NCc1ccc(N2CCOCC2)cc1)Nc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-55648e4dd72e4918928f020267c3f81b
CC1CNCC(C)O1.N#Cc1ccc(F)cc1>>CC1CN(c2ccc(CN)cc2)CC(C)O1
FC1=CC=C(C#N)C=C1.CC1CNCC(O1)C>>CC1CN(CC(O1)C)C1=CC=C(C=C1)CN
[CH3:1][CH:2]1[CH2:3][NH:4][CH2:13][CH:14]([CH3:15])[O:16]1.F[c:5]1[cH:6][cH:7][c:8]([C:9]#[N:10])[cH:11][cH:12]1>>[CH3:1][CH:2]1[CH2:3][N:4]([c:5]2[cH:6][cH:7][c:8]([CH2:9][NH2:10])[cH:11][cH:12]2)[CH2:13][CH:14]([CH3:15])[O:16]1
CC1CNCC(C)O1.N#Cc1ccc(F)cc1
CC1CN(c2ccc(CN)cc2)CC(C)O1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
bb2821dd35ce6e07ed9e7459ce7cc81854777a952694d10cc051b50745e098b9
8974feeb75b9b5e4f2e6d12ce58009881c023f2cc77ffb861190d06c60e864aa
c1ccc(N2CCOCC2)cc1
F-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](-[C;H0;D2;+0:5]#[N;H0;D1;+0:6]):[c:7]:[c:8]:1.[#8:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[NH2;D1;+0:6]-[CH2;D2;+0:5]-[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:12]2-[C:11]-[C:10]-[#8:9]-[C:14]-[C:13]-2):[c:8]:[c:7]:1
null
[]
null
null
null
null
4-Fluorobenzonitrile and 2,6-dimethylmorpholine were processed as described in Examples 66A and 66B to provide the title compound. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Nitrile.Secondary amine
Primary amine.Tertiary amine
C1COCCN1.c1ccccc1
C1COCC[NH]1.c1ccccc1
C1COCC[NH]1.c1ccccc1
Other
null
null
null
CC1CNCC(C)O1.N#Cc1ccc(F)cc1>>CC1CN(c2ccc(CN)cc2)CC(C)O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a13c289538cb4cf1970503aeab75eba8
CC1CN(c2ccc(CN)cc2)CC(C)O1.O=C=Nc1cccc2cnccc12>>CC1CN(c2ccc(CNC(=O)Nc3cccc4cnccc34)cc2)CC(C)O1
CC1CN(CC(O1)C)C1=CC=C(C=C1)CN.N(=C=O)C1=C2C=CN=CC2=CC=C1>>CC1CN(CC(O1)C)C1=CC=C(C=C1)CNC(=O)NC1=C2C=CN=CC2=CC=C1
[CH3:1][CH:2]1[CH2:3][N:4]([c:5]2[cH:6][cH:7][c:8]([CH2:9][NH2:10])[cH:24][cH:25]2)[CH2:26][CH:27]([CH3:28])[O:29]1.[C:11](=[O:12])=[N:13][c:14]1[cH:15][cH:16][cH:17][c:18]2[cH:19][n:20][cH:21][cH:22][c:23]12>>[CH3:1][CH:2]1[CH2:3][N:4]([c:5]2[cH:6][cH:7][c:8]([CH2:9][NH:10][C:11](=[O:12])[NH:13][c:14]3[cH:15][cH:16][c...
CC1CN(c2ccc(CN)cc2)CC(C)O1.O=C=Nc1cccc2cnccc12
CC1CN(c2ccc(CNC(=O)Nc3cccc4cnccc34)cc2)CC(C)O1
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccc(N2CCOCC2)cc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[C:2]-[c:3].[O;D1;H0:4]=[C;H0;D2;+0:5]=[N;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[O;D1;H0:4]=[C;H0;D3;+0:5](-[NH;D2;+0:1]-[C:2]-[c:3])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]
null
[]
null
null
null
null
The product from Example 67A and the product from Example 61A were processed as described in Example 66C to provide a waxy material which was purified by chromatography (95:5 CH2Cl2—MeOH, eluant) to provide the title compound as a white solid. The corresponding di-hydrochloride salt was prepared using methanolic HCl. 1...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
C1COCC[NH]1.c1ccccc1.c1ccc2cnccc2c1
null
null
null
null
CC1CN(c2ccc(CN)cc2)CC(C)O1.O=C=Nc1cccc2cnccc12>>CC1CN(c2ccc(CNC(=O)Nc3cccc4cnccc34)cc2)CC(C)O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-50ac4b0f356f49b4ae8d04d06aaeaf3c
Clc1ccc(N2CCNCC2)cc1Cl.O=C=Nc1cccc2cnccc12>>O=C(Nc1cccc2cnccc12)N1CCN(c2ccc(Cl)c(Cl)c2)CC1
ClC=1C=C(C=CC1Cl)N1CCNCC1.N(=C=O)C1=C2C=CN=CC2=CC=C1>>ClC=1C=C(C=CC1Cl)N1CCN(CC1)C(=O)NC1=C2C=CN=CC2=CC=C1
[NH:14]1[CH2:15][CH2:16][N:17]([c:18]2[cH:19][cH:20][c:21]([Cl:22])[c:23]([Cl:24])[cH:25]2)[CH2:26][CH2:27]1.[O:1]=[C:2]=[N:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12)[N:14]1[CH2:15][CH2:16][N:17]([c:18]2[cH:19][...
Clc1ccc(N2CCNCC2)cc1Cl.O=C=Nc1cccc2cnccc12
O=C(Nc1cccc2cnccc12)N1CCN(c2ccc(Cl)c(Cl)c2)CC1
null
null
C(C)OCC
Acylation
Urea synthesis via isocyanate and secondary amine
6c56e6fc0929cf5b2c535d5ee3915e354a1b28cb53e352800366a2a7d763c4a8
5272a383a93723269f1934f97993b0175b43cd993bcdf2f45add1dbb852d1e09
O=C(Nc1cccc2cnccc12)N1CCN(c2ccccc2)CC1
[#7:1]1-[C:2]-[C:3]-[NH;D2;+0:4]-[C:5]-[C:6]-1.[O;D1;H0:7]=[C;H0;D2;+0:8]=[N;H0;D2;+0:9]-[c:10](:[c:11]):[c:12]>>[O;D1;H0:7]=[C;H0;D3;+0:8](-[NH;D2;+0:9]-[c:10](:[c:11]):[c:12])-[N;H0;D3;+0:4]1-[C:3]-[C:2]-[#7:1]-[C:6]-[C:5]-1
80
[{"value": 80.0, "product": "ClC=1C=C(C=CC1Cl)N1CCN(CC1)C(=O)NC1=C2C=CN=CC2=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
1-(3,4-Dichlorophenyl)piperazine (1280 mg, 5.55 mmol) in diethyl ether (30 mL) was treated with the product from Example 61A (˜40 mL). The mixture was filtered, the filter cake washed with diethyl ether, and dried under reduced pressure to provide the title compound as a white solid (1.78 g, 80%). 1H NMR (300 MHz, DMSO...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Secondary amine
Urea
C1CNCC[NH]1
C1C[NH]CC[NH]1
c1ccc2cnccc2c1.C1C[NH]CC[NH]1.c1ccccc1
null
C(C)OCC
null
null
Clc1ccc(N2CCNCC2)cc1Cl.O=C=Nc1cccc2cnccc12>C(C)OCC>O=C(Nc1cccc2cnccc12)N1CCN(c2ccc(Cl)c(Cl)c2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c8421b9e4bc34d96b0274bd79553161f
Brc1cccc2cnccc12.CCOC(=O)C(=O)OCC>>CCOC(=O)C(=O)c1cccc2cnccc12
[NH4+].[Cl-].C(C(=O)OCC)(=O)OCC.BrC1=C2C=CN=CC2=CC=C1.C(CCC)[Li]>>C1=NC=CC2=C(C=CC=C12)C(C(=O)OCC)=O
Br[c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][n:14][cH:15][cH:16][c:17]12.CCO[C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])=[O:7]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6](=[O:7])[c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][n:14][cH:15][cH:16][c:17]12
Brc1cccc2cnccc12.CCOC(=O)C(=O)OCC
CCOC(=O)C(=O)c1cccc2cnccc12
null
null
C1CCOC1
C-C Coupling
Ester and halide to ketone
c2f0786450e86e8f47917ca1d9f974bf315ab7618b97528e08a0299591acc115
dd03ca4e617545414fae7e22c410ecd4f78e4fd10d5a86bce7e36a4a1d0f1e9d
c1ccc2cnccc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.C-C-O-[C;H0;D3;+0:10](=[O;D1;H0:11])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:15]-[#8:14]-[C:12](=[O;D1;H0:13])-[C;H0;D3;+0:10](=[O;D1;H0:11])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
35.2
[{"value": 35.0, "product": "C1=NC=CC2=C(C=CC=C12)C(C(=O)OCC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 35.2, "product": "C1=NC=CC2=C(C=CC=C12)C(C(=O)OCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
The product from Example 57A (11.80 g, 56.6 mmol) in THF (200 mL) at −78° C. was treated with n-butyllithium (30 mL, 75.0 mmol, 2.5M in hexanes) dropwise. After 30 minutes, the mixture was treated with diethyl oxalate (25.0 mL, 184 mmol). After 20 minutes, the solution was allowed to warm to room temperature and was tr...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ester.Ester
Ketone
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HBr
C1CCOC1
null
0.5
Brc1cccc2cnccc12.CCOC(=O)C(=O)OCC>C1CCOC1>CCOC(=O)C(=O)c1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f81aba286c6c4712992f65f7c6a08880
CC(=O)Cl.CCOC(=O)C(O)c1cccc2cnccc12>>CCOC(=O)C(OC(C)=O)c1cccc2cnccc12
OC(C(=O)OCC)C1=C2C=CN=CC2=CC=C1.C(C)(=O)Cl>>C(C)(=O)OC(C(=O)OCC)C1=C2C=CN=CC2=CC=C1
Cl[C:8]([CH3:9])=[O:10].[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([OH:7])[c:11]1[cH:12][cH:13][cH:14][c:15]2[cH:16][n:17][cH:18][cH:19][c:20]12>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([O:7][C:8]([CH3:9])=[O:10])[c:11]1[cH:12][cH:13][cH:14][c:15]2[cH:16][n:17][cH:18][cH:19][c:20]12
CC(=O)Cl.CCOC(=O)C(O)c1cccc2cnccc12
CCOC(=O)C(OC(C)=O)c1cccc2cnccc12
null
null
N1=CC=CC=C1
Acylation
Schotten-Baumann to ester
27b76e29491fa7db5375755e15223de884a194f57a493147db0b5495ea981908
d47ab90ace9b5dcd818151c10aae400dcf599f5a3476072b8dfedc474e97c335
c1ccc2cnccc2c1
Cl-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[C:4]-[#8:5]-[C:6](=[O;D1;H0:7])-[C:8](-[OH;D1;+0:9])-[c:10]>>[C:4]-[#8:5]-[C:6](=[O;D1;H0:7])-[C:8](-[c:10])-[O;H0;D2;+0:9]-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3]
67.2
[{"value": 67.0, "product": "C(C)(=O)OC(C(=O)OCC)C1=C2C=CN=CC2=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 67.2, "product": "C(C)(=O)OC(C(=O)OCC)C1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
The product of Example 70B (1.0202 g, 4.41 mmol) in pyridine (15 mL) was treated with acetyl chloride (0.35 mL, 4.92 mmol) dropwise. The solution was stirred at room temperature for 4 hours and concentrated under reduced pressure. The residue was purified by column chromatography (2% methanol/CH2CH2) to provide the tit...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary alcohol
Ester
null
null
c1ccc2cnccc2c1
HCl
N1=CC=CC=C1
null
4
CC(=O)Cl.CCOC(=O)C(O)c1cccc2cnccc12>N1=CC=CC=C1>CCOC(=O)C(OC(C)=O)c1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2cd6e83b53a34d02a19b609fd0150a3d
CCOC(=O)C(OC(C)=O)c1cccc2cnccc12>>CCOC(=O)Cc1cccc2cnccc12
C(C)(=O)OC(C(=O)OCC)C1=C2C=CN=CC2=CC=C1>>C1=NC=CC2=C(C=CC=C12)CC(=O)OCC
CC(=O)O[CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:7]1[cH:8][cH:9][cH:10][c:11]2[cH:12][n:13][cH:14][cH:15][c:16]12>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[cH:12][n:13][cH:14][cH:15][c:16]12
CCOC(=O)C(OC(C)=O)c1cccc2cnccc12
CCOC(=O)Cc1cccc2cnccc12
null
null
C(C)O
Reduction
OtherReaction
33f176f6ce02426b2726e71e3c19f64673952a2b50dd48518b89a08efe25965b
b45711df98eaf2a3f54e3027da3f1b57580ab2f6d54e9ac2a56731961e64969a
c1ccc2cnccc2c1
C-C(=O)-O-[CH;D3;+0:1](-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5])-[c:6](:[c:7]):[c:8]>>[C:5]-[#8:4]-[C:2](=[O;D1;H0:3])-[CH2;D2;+0:1]-[c:6](:[c:7]):[c:8]
82.6
[{"value": 67.0, "product": "C1=NC=CC2=C(C=CC=C12)CC(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.6, "product": "C1=NC=CC2=C(C=CC=C12)CC(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
6
HOUR
The product of Example 70C (1.43 g, 5.23 mmol) in absolute ethanol (200 mL) was treated with dry 10% Pd/C (0.122 g) and triethylamine (10.4 mL). The reaction mixture was stirred at 60° C. for 6 hours under H2 (60 psi), filtered and the filtrate concentrated under reduced pressure. The residue was purified by column chr...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Ester
null
null
c1ccc2cnccc2c1
HO-
C(C)O
60
6
CCOC(=O)C(OC(C)=O)c1cccc2cnccc12>C(C)O>CCOC(=O)Cc1cccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b94a35791cae4b8ea43dc8ab5851d733
CCOC(=O)Cc1cccc2cnccc12.NCc1ccc(C(F)(F)F)cc1>>O=C(Cc1cccc2cnccc12)NCc1ccc(C(F)(F)F)cc1
Cl.C1=NC=CC2=C(C=CC=C12)CC(=O)OCC.C[Al](C)C.[NH4+].[OH-].FC(C1=CC=C(CN)C=C1)(F)F>>C1=NC=CC2=C(C=CC=C12)CC(=O)NCC1=CC=C(C=C1)C(F)(F)F
CCO[C:2](=[O:1])[CH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12.[NH2:14][CH2:15][c:16]1[cH:17][cH:18][c:19]([C:20]([F:21])([F:22])[F:23])[cH:24][cH:25]1>>[O:1]=[C:2]([CH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][cH:12][c:13]12)[NH:14][CH2:15][c:16]1[cH:17][cH:18][c:19]([C:20]([F:21])(...
CCOC(=O)Cc1cccc2cnccc12.NCc1ccc(C(F)(F)F)cc1
O=C(Cc1cccc2cnccc12)NCc1ccc(C(F)(F)F)cc1
null
null
ClCCl.O.C(Cl)Cl
Acylation
Aminolysis of esters
04c54ce22aa9bc0cea0de3d900446bcab51cf02bebeb606fa788a47dcd0e37ff
4335147c9ad02004b7c12428d7eac0b2e7e0e2017adc471d01c387239de8017d
O=C(Cc1cccc2cnccc12)NCc1ccccc1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4].[NH2;D1;+0:5]-[C:6]-[c:7]>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[C:3]-[c:4])-[NH;D2;+0:5]-[C:6]-[c:7]
37
[{"value": 37.0, "product": "C1=NC=CC2=C(C=CC=C12)CC(=O)NCC1=CC=C(C=C1)C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 36.9, "product": "C1=NC=CC2=C(C=CC=C12)CC(=O)NCC1=CC=C(C=C1)C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
The product from Example 70D (0.207 g, 0.96 mmol) in dichloromethane (10 mL) was treated with trimethylaluminum (1 mL, 2.0 mmol, 2M in toluene) dropwise. After 30 minutes, the mixture was teated with 4-(trifluoromethyl)benzylamine (0.350 g, 2.0 mmol) in dichloromethane (2 mL) and then refluxed for 16 hours. The reactio...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Secondary amide
null
null
c1ccc2cnccc2c1.c1ccccc1
HO-
ClCCl.O.C(Cl)Cl
null
0.5
CCOC(=O)Cc1cccc2cnccc12.NCc1ccc(C(F)(F)F)cc1>ClCCl.O.C(Cl)Cl>O=C(Cc1cccc2cnccc12)NCc1ccc(C(F)(F)F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9178f29f1218402098e6fa03da8337ae
COC(=O)c1cc2ccccc2cn1.O=[N+]([O-])[O-]>>COC(=O)c1cc2c([N+](=O)[O-])cccc2cn1
C1=NC(=CC2=CC=CC=C12)C(=O)OC.[N+](=O)([O-])[O-].[Na+]>>[N+](=O)([O-])C1=C2C=C(N=CC2=CC=C1)C(=O)OC
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]2[cH:8][cH:12][cH:13][cH:14][c:15]2[cH:16][n:17]1.[O-][N+:9](=[O:10])[O-:11]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]2[c:8]([N+:9](=[O:10])[O-:11])[cH:12][cH:13][cH:14][c:15]2[cH:16][n:17]1
COC(=O)c1cc2ccccc2cn1.O=[N+]([O-])[O-]
COC(=O)c1cc2c([N+](=O)[O-])cccc2cn1
null
null
OS(=O)(=O)O
Functional Group Addition
Aromatic nitration with NO3 salt
dcb421e65a8922cd9594f5567e7ba6ab06a8bfe0650592bab8d9da3689fbb53d
ddce49825c02b8965f10c8d99e3c841d26e1f136da6037b417c09313e6d73097
c1ccc2cnccc2c1
[O-]-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3].[c:4]:[c:5]:[cH;D2;+0:6]:[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1>>[O;-;D1;H0:2]-[N+;H0;D3:1](=[O;D1;H0:3])-[c;H0;D3;+0:6](:[c:5]:[c:4]):[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1
96.2
[{"value": 96.0, "product": "[N+](=O)([O-])C1=C2C=C(N=CC2=CC=C1)C(=O)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.2, "product": "[N+](=O)([O-])C1=C2C=C(N=CC2=CC=C1)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
Methyl isoquinoline-3-carboxylate (9.58 g, 51.2 mmol) in concentrated H2SO4 (100 mL) at 0° C. was treated with sodium nitrate (4.79 g, 56.4 mmol) in small portions such that the temperature was maintained below 5° C. Ten minutes after addition was complete, the reaction mixture was allowed to warm to room temperature a...
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HO-
OS(=O)(=O)O
null
2
COC(=O)c1cc2ccccc2cn1.O=[N+]([O-])[O-]>OS(=O)(=O)O>COC(=O)c1cc2c([N+](=O)[O-])cccc2cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-01fb787146f347a1af791d906562fe79
COC(=O)c1cc2c([N+](=O)[O-])cccc2cn1>>COC(=O)c1cc2c(N)cccc2cn1
[N+](=O)([O-])C1=C2C=C(N=CC2=CC=C1)C(=O)OC.CO.C(Cl)Cl>>NC1=C2C=C(N=CC2=CC=C1)C(=O)OC
O=[N+:9]([O-])[c:8]1[c:7]2[cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[n:15][cH:14][c:13]2[cH:12][cH:11][cH:10]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]2[c:8]([NH2:9])[cH:10][cH:11][cH:12][c:13]2[cH:14][n:15]1
COC(=O)c1cc2c([N+](=O)[O-])cccc2cn1
COC(=O)c1cc2c(N)cccc2cn1
null
[Fe]
C(C)(=O)O.O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2cnccc2c1
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
16
HOUR
The product of Example 71A (10.33 g, 44.5 mmol) in acetic acid/water (3/1) (320 mL) was treated with iron powder (5.06 g, 90.7 mmol). After stirring for 16 hours at room temperature, the reaction mixture was filtered the filtrate concentrated under reduced pressure to approximately half the original volume. The mixture...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2cnccc2c1
Other
[Fe].C(C)(=O)O.O
null
16
COC(=O)c1cc2c([N+](=O)[O-])cccc2cn1>[Fe].C(C)(=O)O.O>COC(=O)c1cc2c(N)cccc2cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fa24ed6b072c4b2588f2110a59e2631e
COC(=O)c1cc2c(N)cccc2cn1.O=C=NCc1ccc(Br)cc1>>COC(=O)c1cc2c(NC(=O)NCc3ccc(Br)cc3)cccc2cn1
NC1=C2C=C(N=CC2=CC=C1)C(=O)OC.C1(=CC=CC=C1)C.BrC1=CC=C(C=C1)CN=C=O>>BrC1=CC=C(CNC(=O)NC2=C3C=C(N=CC3=CC=C2)C(=O)OC)C=C1
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]2[c:8]([NH2:9])[cH:21][cH:22][cH:23][c:24]2[cH:25][n:26]1.[C:10](=[O:11])=[N:12][CH2:13][c:14]1[cH:15][cH:16][c:17]([Br:18])[cH:19][cH:20]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]2[c:8]([NH:9][C:10](=[O:11])[NH:12][CH2:13][c:14]3[cH:15][cH:16][c:17]([Br:18])[cH:19][cH:20]3)...
COC(=O)c1cc2c(N)cccc2cn1.O=C=NCc1ccc(Br)cc1
COC(=O)c1cc2c(NC(=O)NCc3ccc(Br)cc3)cccc2cn1
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:7]-[C:8]-[c:9])-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]
85.3
[{"value": 85.0, "product": "BrC1=CC=C(CNC(=O)NC2=C3C=C(N=CC3=CC=C2)C(=O)OC)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 85.3, "product": "BrC1=CC=C(CNC(=O)NC2=C3C=C(N=CC3=CC=C2)C(=O)OC)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
The product of Example 71B (0.156 g, 0.77 mmol) in THF:toluene (10 mL, 1:1) was treated with a solution of 1-bromo-4-(isocyanatomethyl)benzene (0.201 g, 0.95 mmol) in THF (1.0 mL). After stirring for 16 hours at room temperature, the reaction mixture was concentrated under reduced pressure and the residue was triturate...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
C1CCOC1
null
16
COC(=O)c1cc2c(N)cccc2cn1.O=C=NCc1ccc(Br)cc1>C1CCOC1>COC(=O)c1cc2c(NC(=O)NCc3ccc(Br)cc3)cccc2cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0698f79948cc4b37adf3f01e3952f75c
COC(=O)c1cc2c(N)cccc2cn1.O=C=NCc1ccc(Cl)cc1Cl>>COC(=O)c1cc2c(NC(=O)NCc3ccc(Cl)cc3Cl)cccc2cn1
NC1=C2C=C(N=CC2=CC=C1)C(=O)OC.C1(=CC=CC=C1)C.ClC1=C(C=CC(=C1)Cl)CN=C=O>>ClC1=C(CNC(=O)NC2=C3C=C(N=CC3=CC=C2)C(=O)OC)C=CC(=C1)Cl
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]2[c:8]([NH2:9])[cH:22][cH:23][cH:24][c:25]2[cH:26][n:27]1.[C:10](=[O:11])=[N:12][CH2:13][c:14]1[cH:15][cH:16][c:17]([Cl:18])[cH:19][c:20]1[Cl:21]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]2[c:8]([NH:9][C:10](=[O:11])[NH:12][CH2:13][c:14]3[cH:15][cH:16][c:17]([Cl:18])[cH:19][c:...
COC(=O)c1cc2c(N)cccc2cn1.O=C=NCc1ccc(Cl)cc1Cl
COC(=O)c1cc2c(NC(=O)NCc3ccc(Cl)cc3Cl)cccc2cn1
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:7]-[C:8]-[c:9])-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]
73
[{"value": 73.0, "product": "ClC1=C(CNC(=O)NC2=C3C=C(N=CC3=CC=C2)C(=O)OC)C=CC(=C1)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.6, "product": "ClC1=C(CNC(=O)NC2=C3C=C(N=CC3=CC=C2)C(=O)OC)C=CC(=C1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
The product of Example 71B (0.156 g, 0.77 mmol) in THF:toluene (10 mL, 1:1) was treated with a solution of 2,4-dichloro-1-(isocyanatomethyl)benzene (0.195 g, 0.97 mmol) in THF (1.0 mL). After stirring for 16 hours at room temperature, the reaction mixture was concentrated under reduced pressure and the residue was trit...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
C1CCOC1
null
16
COC(=O)c1cc2c(N)cccc2cn1.O=C=NCc1ccc(Cl)cc1Cl>C1CCOC1>COC(=O)c1cc2c(NC(=O)NCc3ccc(Cl)cc3Cl)cccc2cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c15f0d07ca94425cb81ba6badf1891b1
BrBr.Nc1cccc2cnccc12>>Nc1ccc(Br)c2cnccc12
[OH-].[Na+].NC1=C2C=CN=CC2=CC=C1.[Cl-].[Cl-].[Cl-].[Al+3].BrBr>>BrC1=CC=C(C=2C=CN=CC12)N
Br[Br:6].[NH2:1][c:2]1[cH:3][cH:4][cH:5][c:7]2[cH:8][n:9][cH:10][cH:11][c:12]12>>[NH2:1][c:2]1[cH:3][cH:4][c:5]([Br:6])[c:7]2[cH:8][n:9][cH:10][cH:11][c:12]12
BrBr.Nc1cccc2cnccc12
Nc1ccc(Br)c2cnccc12
null
null
C(C)(=O)OCC
Functional Group Interconversion
Bromination
dd766f53887400b5e199d60af04f01509e5613a22375639572626e4514c9ae8d
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc2cnccc2c1
Br-[Br;H0;D1;+0:1].[c:2]:[#7;a:3]:[c:4]:[c:5](:[c:6]):[cH;D2;+0:7]:[c:8]:[c:9]>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:5](:[c:6]):[c:4]:[#7;a:3]:[c:2]
69.7
[{"value": 35.0, "product": "BrC1=CC=C(C=2C=CN=CC12)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 69.7, "product": "BrC1=CC=C(C=2C=CN=CC12)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
2
HOUR
5-Aminoisoquinoline (5.50 g, 38.1 mmol) and aluminium trichloride (15.1 g, 113 mmol) were combined and heated at 80° C. in a 3-necked flask equipped with a dropping funnel, stirrer bar, needle and sintered glass tube. Bromine (3.04 g, 19.05 mmol) was dripped onto the sintered glass funnel and the vapour diffused onto t...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HBr
C(C)(=O)OCC
80
2
BrBr.Nc1cccc2cnccc12>C(C)(=O)OCC>Nc1ccc(Br)c2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2dd9c98cd52743aeb03c3f220dba9b0f
Nc1ccc(Br)c2cnccc12.O=C=NCc1ccc(Cl)cc1Cl>>O=C(NCc1ccc(Cl)cc1Cl)Nc1ccc(Br)c2cnccc12
BrC1=CC=C(C=2C=CN=CC12)N.C1(=CC=CC=C1)C.ClC1=C(C=CC(=C1)Cl)CN=C=O>>BrC=1C=CC(=C2C=CN=CC12)NC(=O)NCC1=C(C=C(C=C1)Cl)Cl
[NH2:13][c:14]1[cH:15][cH:16][c:17]([Br:18])[c:19]2[cH:20][n:21][cH:22][cH:23][c:24]12.[O:1]=[C:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[cH:10][c:11]1[Cl:12]>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[cH:10][c:11]1[Cl:12])[NH:13][c:14]1[cH:15][cH:16][c:17]([Br:18])[c:19]2[cH:20][n:21][cH:22][cH:23]...
Nc1ccc(Br)c2cnccc12.O=C=NCc1ccc(Cl)cc1Cl
O=C(NCc1ccc(Cl)cc1Cl)Nc1ccc(Br)c2cnccc12
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[NH;D2;+0:7]-[C:8]-[c:9]
80.5
[{"value": 78.0, "product": "BrC=1C=CC(=C2C=CN=CC12)NC(=O)NCC1=C(C=C(C=C1)Cl)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 80.5, "product": "BrC=1C=CC(=C2C=CN=CC12)NC(=O)NCC1=C(C=C(C=C1)Cl)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
The product from Example 73A (120 mg, 0.52 mmol) in THF:toluene (1.4, 5 mL) was treated with a solution of 2,4-dichloro-1-(isocyanatomethyl)benzene (108 mg, 0.52 mmol) in THF (0.5 mL). After stirring for 16 hours at room temperature, the mixture was filtered and the filter cake dried under reduced pressure to provide t...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
C1CCOC1
null
16
Nc1ccc(Br)c2cnccc12.O=C=NCc1ccc(Cl)cc1Cl>C1CCOC1>O=C(NCc1ccc(Cl)cc1Cl)Nc1ccc(Br)c2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-64d581fdecb8443b8ea98f84eff7dba9
Nc1ccc(Br)c2cnccc12.O=C=NCc1ccc(F)cc1>>O=C(NCc1ccc(F)cc1)Nc1ccc(Br)c2cnccc12
FC1=CC=C(C=C1)CN=C=O.BrC1=CC=C(C=2C=CN=CC12)N>>BrC=1C=CC(=C2C=CN=CC12)NC(=O)NCC1=CC=C(C=C1)F
[NH2:12][c:13]1[cH:14][cH:15][c:16]([Br:17])[c:18]2[cH:19][n:20][cH:21][cH:22][c:23]12.[O:1]=[C:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([F:9])[cH:10][cH:11]1>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([F:9])[cH:10][cH:11]1)[NH:12][c:13]1[cH:14][cH:15][c:16]([Br:17])[c:18]2[cH:19][n:20][cH:21][cH:22][c:23]12
Nc1ccc(Br)c2cnccc12.O=C=NCc1ccc(F)cc1
O=C(NCc1ccc(F)cc1)Nc1ccc(Br)c2cnccc12
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[NH;D2;+0:7]-[C:8]-[c:9]
null
[]
null
null
null
null
The title compound was prepared using 1-fluoro-4-(isocyanatomethyl)benzene, the product of Example 73A and the procedure described in Example 73B (white solid, 108 mg, 65%) MS (ESI+) m/z 376 (M+H)+; MS (ESI−) m/z 374 (M−H)−; 1H NMR (DMSO-d6, 300 MHz) δ 4.35 (d, 5.8, 2H), 7.12 (m, 1H), 7.18 (m, 2H), 7.40 (m, 1H), 7.91 (...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
null
null
null
Nc1ccc(Br)c2cnccc12.O=C=NCc1ccc(F)cc1>>O=C(NCc1ccc(F)cc1)Nc1ccc(Br)c2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fc1f90ba027d43989e6d6e60ee769702
Nc1ccc(Br)c2cnccc12.O=C=NCc1cccc(F)c1>>O=C(NCc1cccc(F)c1)Nc1ccc(Br)c2cnccc12
FC1=CC(=CC=C1)CN=C=O.BrC1=CC=C(C=2C=CN=CC12)N>>BrC=1C=CC(=C2C=CN=CC12)NC(=O)NCC1=CC(=CC=C1)F
[NH2:12][c:13]1[cH:14][cH:15][c:16]([Br:17])[c:18]2[cH:19][n:20][cH:21][cH:22][c:23]12.[O:1]=[C:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][cH:8][c:9]([F:10])[cH:11]1>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][cH:8][c:9]([F:10])[cH:11]1)[NH:12][c:13]1[cH:14][cH:15][c:16]([Br:17])[c:18]2[cH:19][n:20][cH:21][cH:22][c:23]12
Nc1ccc(Br)c2cnccc12.O=C=NCc1cccc(F)c1
O=C(NCc1cccc(F)c1)Nc1ccc(Br)c2cnccc12
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[NH;D2;+0:7]-[C:8]-[c:9]
null
[]
null
null
null
null
The title compound was prepared using 1-fluoro-3-(isocyanatomethyl)benzene, the product of Example 73A and the procedure described in Example 73 (white solid, 108 mg, 65%). MS (ESI+) m/z 376 (M+H)+; MS (ESI−) m/z 374 (M−H)−; 1H NMR (DMSO-d6, 300 MHz) δ 4.39 (d, 5.8, 2H), 7.09 (m, 1H), 7.17 (m, 2H), 7.40 (m, 1H), 7.91 (...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
null
null
null
Nc1ccc(Br)c2cnccc12.O=C=NCc1cccc(F)c1>>O=C(NCc1cccc(F)c1)Nc1ccc(Br)c2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-58ebfe9b7cb34e039a7f12d2ebcbb5ef
CC(C)(C(=O)O)c1ccc(Cl)cc1.O=S(Cl)Cl>>CC(C)(C(=O)Cl)c1ccc(Cl)cc1
ClC1=CC=C(C=C1)C(C(=O)O)(C)C.S(=O)(Cl)Cl>>ClC1=CC=C(C=C1)C(C(=O)Cl)(C)C
O[C:4]([C:2]([CH3:1])([CH3:3])[c:7]1[cH:8][cH:9][c:10]([Cl:11])[cH:12][cH:13]1)=[O:5].O=S(Cl)[Cl:6]>>[CH3:1][C:2]([CH3:3])([C:4](=[O:5])[Cl:6])[c:7]1[cH:8][cH:9][c:10]([Cl:11])[cH:12][cH:13]1
CC(C)(C(=O)O)c1ccc(Cl)cc1.O=S(Cl)Cl
CC(C)(C(=O)Cl)c1ccc(Cl)cc1
null
null
CCCCCC.C1(=CC=CC=C1)C
Functional Group Interconversion
Alcohol to chloride_SOCl2
c301c14a9dcd0670d52e8b77396cbe7fd8edeedd757bc43f4162ade1fc52fc93
787f545db5dc0b29dde55b5fbed7db8625b8055f49327f97ed4d83cc47c3af1d
c1ccccc1
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[c:7]>>[C;D1;H3:5]-[C:4](-[C;D1;H3:6])(-[c:7])-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3]
98
[{"value": 98.0, "product": "ClC1=CC=C(C=C1)C(C(=O)Cl)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.4, "product": "ClC1=CC=C(C=C1)C(C(=O)Cl)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
2-(4-Chlorophenyl)-2-methylpropanoic acid (3.85 g, 19.4 mmol) in toluene (5 mL) was treated with thionyl chloride (5.00 g, 3.1 mL) and heated at 80° C. for 2 hours. The cooled solution was concentrated under reduced pressure to provide a yellow oil containing a crystalline residue. The mixture was dissolved in hexane, ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Acyl halide
null
null
c1ccccc1
HCl
CCCCCC.C1(=CC=CC=C1)C
80
null
CC(C)(C(=O)O)c1ccc(Cl)cc1.O=S(Cl)Cl>CCCCCC.C1(=CC=CC=C1)C>CC(C)(C(=O)Cl)c1ccc(Cl)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-db14f5bfc589491191cd8ac60651eaa1
CC(C)(C(=O)Cl)c1ccc(Cl)cc1>>CC(C)(N=C=O)c1ccc(Cl)cc1
ClC1=CC=C(C=C1)C(C(=O)Cl)(C)C.[N-]=[N+]=[N-].[Na+].CC(=O)C>>ClC1=CC=C(C=C1)C(C)(C)N=C=O
Cl[C:5]([C:2]([CH3:1])([CH3:3])[c:7]1[cH:8][cH:9][c:10]([Cl:11])[cH:12][cH:13]1)=[O:6]>>[CH3:1][C:2]([CH3:3])([N:4]=[C:5]=[O:6])[c:7]1[cH:8][cH:9][c:10]([Cl:11])[cH:12][cH:13]1
CC(C)(C(=O)Cl)c1ccc(Cl)cc1
CC(C)(N=C=O)c1ccc(Cl)cc1
null
null
O
Functional Group Interconversion
OtherReaction
fbf2339641ff0cdb5e15752f21553572109b22d0761d12b2dad0b963d5d29fa7
cc08743a6a6e57f91530e729ed5783f6b5577caba801cdc96f6a1c4a9df32591
c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C;H0;D4;+0:3](-[C;D1;H3:4])(-[C;D1;H3:5])-[c:6](:[c:7]):[c:8]>>[C;D1;H3:4]-[C;H0;D4;+0:3](-[C;D1;H3:5])(-[#7:9]=[C;H0;D2;+0:1]=[O;D1;H0:2])-[c:6](:[c:7]):[c:8]
96
[{"value": 96.0, "product": "ClC1=CC=C(C=C1)C(C)(C)N=C=O", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
The product of Example 76A (4.00 g, 19.4 mmol) in acetone (9 mL) at 0° C. was treated with a solution of sodium azide (1.27 g) in water (9 mL) dropwise over 15 minutes. After stirring for 30 minutes at 0° C., the mixture was extracted with toluene (20 mL). The organic extract was dried with MgSO4, filtered, and the fil...
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Isocyanate
null
null
c1ccccc1
null
O
0
0.5
CC(C)(C(=O)Cl)c1ccc(Cl)cc1>O>CC(C)(N=C=O)c1ccc(Cl)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b1299c6fa1584a449bf4be13c0a1832e
CC(C)(N=C=O)c1ccc(Cl)cc1.Nc1cccc2cnccc12>>CC(C)(NC(=O)Nc1cccc2cnccc12)c1ccc(Cl)cc1
NC1=C2C=CN=CC2=CC=C1.ClC1=CC=C(C=C1)C(C)(C)N=C=O>>ClC1=CC=C(C=C1)C(C)(C)NC(=O)NC1=C2C=CN=CC2=CC=C1
[CH3:1][C:2]([CH3:3])([N:4]=[C:5]=[O:6])[c:18]1[cH:19][cH:20][c:21]([Cl:22])[cH:23][cH:24]1.[NH2:7][c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][n:14][cH:15][cH:16][c:17]12>>[CH3:1][C:2]([CH3:3])([NH:4][C:5](=[O:6])[NH:7][c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][n:14][cH:15][cH:16][c:17]12)[c:18]1[cH:19][cH:20][c:21]([Cl:22]...
CC(C)(N=C=O)c1ccc(Cl)cc1.Nc1cccc2cnccc12
CC(C)(NC(=O)Nc1cccc2cnccc12)c1ccc(Cl)cc1
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[C;D1;H3:1]-[C:2](-[C;D1;H3:3])(-[c:4])-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7].[NH2;D1;+0:8]-[c:9](:[c:10]):[c:11]>>[C;D1;H3:1]-[C:2](-[C;D1;H3:3])(-[c:4])-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:8]-[c:9](:[c:10]):[c:11]
34
[{"value": 34.0, "product": "ClC1=CC=C(C=C1)C(C)(C)NC(=O)NC1=C2C=CN=CC2=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared using 5-aminoisoquinoline, the product of Example 76B and the procedure described in Example 73B except that THF was used as solvent. The product was recrystallized from ethyl acetate to provide the title compound as a white solid (840 mg, 34%). MS (ESI+) m/z 355 (M+H)+; MS (ESI−) m/z 35...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccc2cnccc2c1.c1ccccc1
null
C1CCOC1
null
null
CC(C)(N=C=O)c1ccc(Cl)cc1.Nc1cccc2cnccc12>C1CCOC1>CC(C)(NC(=O)Nc1cccc2cnccc12)c1ccc(Cl)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5792bf11df114477af29d7fe662be805
Nc1cccc2cnccc12.O=C(C(F)(F)F)C(F)(F)F>>Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12
NC1=C2C=CN=CC2=CC=C1.O.O.O.O.O.O.FC(C(=O)C(F)(F)F)(F)F>>NC1=C2C=CN=CC2=CC=C1C(C(F)(F)F)(C(F)(F)F)O
[NH2:1][c:2]1[cH:3][cH:14][cH:15][c:16]2[cH:17][n:18][cH:19][cH:20][c:21]12.[C:4](=[O:5])([C:6]([F:7])([F:8])[F:9])[C:10]([F:11])([F:12])[F:13]>>[NH2:1][c:2]1[c:3]([C:4]([OH:5])([C:6]([F:7])([F:8])[F:9])[C:10]([F:11])([F:12])[F:13])[cH:14][cH:15][c:16]2[cH:17][n:18][cH:19][cH:20][c:21]12
Nc1cccc2cnccc12.O=C(C(F)(F)F)C(F)(F)F
Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12
null
C1(=CC=C(C=C1)S(=O)(=O)O)C
null
C-C Coupling
OtherReaction
ddb379ad63d99a5f7ded013bf598cb3b376f94f1ff8e2a4b87fa503953b27a47
454f67ba8644982dc9f605915a0f36178771eadaffb50d3f1e0f17f2b6fdeb10
c1ccc2cnccc2c1
[F;D1;H0:1]-[C:2](-[F;D1;H0:3])(-[F;D1;H0:4])-[C;H0;D3;+0:5](=[O;H0;D1;+0:6])-[C:7](-[F;D1;H0:8])(-[F;D1;H0:9])-[F;D1;H0:10].[N;D1;H2:11]-[c:12](:[c:13]):[cH;D2;+0:14]:[c:15]:[c:16]>>[F;D1;H0:1]-[C:2](-[F;D1;H0:3])(-[F;D1;H0:4])-[C;H0;D4;+0:5](-[OH;D1;+0:6])(-[c;H0;D3;+0:14](:[c:15]:[c:16]):[c:12](-[N;D1;H2:11]):[c:13]...
30
[{"value": 30.0, "product": "NC1=C2C=CN=CC2=CC=C1C(C(F)(F)F)(C(F)(F)F)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 21.0, "product": "NC1=C2C=CN=CC2=CC=C1C(C(F)(F)F)(C(F)(F)F)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
150
CELSIUS
null
null
5-Aminoisoquinoline (288 mg, 2.00 mmol) and p-toluenesulfonic acid (5 mg) were combined and treated with hexafluoroacetone hexahydrate (0.29 mL, 462 mg, 2.10 mmol). The mixture was stirred in a sealed pressure tube and heated to 150° C. for 18 hours. The reaction was allowed to cool to room temperature and partitioned ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Tertiary alcohol
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
null
C1(=CC=C(C=C1)S(=O)(=O)O)C
150
null
Nc1cccc2cnccc12.O=C(C(F)(F)F)C(F)(F)F>C1(=CC=C(C=C1)S(=O)(=O)O)C>Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-419f73c2ccd540af8eda4c2260f31adf
Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12.O=C=NCc1ccc(Br)cc1>>O=C(NCc1ccc(Br)cc1)Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12
BrC1=CC=C(C=C1)CN=C=O.NC1=C2C=CN=CC2=CC=C1C(C(F)(F)F)(C(F)(F)F)O>>BrC1=CC=C(CNC(=O)NC2=C3C=CN=CC3=CC=C2C(C(F)(F)F)(C(F)(F)F)O)C=C1
[NH2:12][c:13]1[c:14]([C:15]([OH:16])([C:17]([F:18])([F:19])[F:20])[C:21]([F:22])([F:23])[F:24])[cH:25][cH:26][c:27]2[cH:28][n:29][cH:30][cH:31][c:32]12.[O:1]=[C:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Br:9])[cH:10][cH:11]1>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Br:9])[cH:10][cH:11]1)[NH:12][c:13]1[c:14]([C...
Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12.O=C=NCc1ccc(Br)cc1
O=C(NCc1ccc(Br)cc1)Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2cnccc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:7]-[C:8]-[c:9]>>[O;D1;H0:5]=[C;H0;D3;+0:6](-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[NH;D2;+0:7]-[C:8]-[c:9]
null
[]
null
null
null
null
The title compound was prepared using 1-bromo-4-(isocyanatomethyl)benzene, the product of Example 77A and the procedure described in Example 73B except that THF was used as solvent (white solid, 840 mg, 34%). MS (ESI+) m/z 376 (M+H)+; MS (ESI−) m/z 374 (M−H)−; 1H NMR (DMSO-d6, 300 MHz) δ 4.35 (d, 5.8, 2H), 7.12 (m, 1H)...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2cnccc2c1
null
C1CCOC1
null
null
Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12.O=C=NCc1ccc(Br)cc1>C1CCOC1>O=C(NCc1ccc(Br)cc1)Nc1c(C(O)(C(F)(F)F)C(F)(F)F)ccc2cnccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2ab03b67d609402ea896932a96ef91f3
Nc1cccc2[nH]ccc12.O=C=NCc1ccc(Br)cc1>>O=C(NCc1ccc(Br)cc1)Nc1cccc2[nH]ccc12
CCCCCC.NC1=C2C=CNC2=CC=C1.BrC1=CC=C(C=C1)CN=C=O>>BrC1=CC=C(CNC(=O)NC2=C3C=CNC3=CC=C2)C=C1
[NH2:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[nH:18][cH:19][cH:20][c:21]12.[O:1]=[C:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Br:9])[cH:10][cH:11]1>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Br:9])[cH:10][cH:11]1)[NH:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[nH:18][cH:19][cH:20][c:21]12
Nc1cccc2[nH]ccc12.O=C=NCc1ccc(Br)cc1
O=C(NCc1ccc(Br)cc1)Nc1cccc2[nH]ccc12
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2[nH]ccc12
[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH2;D1;+0:5]):[c:6].[O;D1;H0:7]=[C;H0;D2;+0:8]=[N;H0;D2;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:8](=[O;D1;H0:7])-[NH;D2;+0:9]-[C:10]-[c:11]):[c:6]
null
[]
null
null
null
null
4-aminoindole (0.13 g, 1 mmol) in THF (3 mL) was treated with 1-bromo-4-(isocyanatomethyl)benzene (0.23 g, 1.1 mmol) for 3 hours at ambient temperature. Hexane was added to the reaction mixture to precipitate 0.26 g of the title compound as a tan solid. mp 198° C.; 1H NMR (300 MHz, DMSO-d6) δ 4.30 (d, 2H), 6.51 (t, 1H)...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
null
C1CCOC1
null
null
Nc1cccc2[nH]ccc12.O=C=NCc1ccc(Br)cc1>C1CCOC1>O=C(NCc1ccc(Br)cc1)Nc1cccc2[nH]ccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-60f6a2e647de494cbda989dfd2269117
Nc1cccc2[nH]ccc12.O=C=NCc1ccc(Cl)c(Cl)c1>>O=C(NCc1ccc(Cl)c(Cl)c1)Nc1cccc2[nH]ccc12
CCCCCC.NC1=C2C=CNC2=CC=C1.ClC1=C(C=C(C=C1)CN=C=O)Cl>>ClC=1C=C(CNC(=O)NC2=C3C=CNC3=CC=C2)C=CC1Cl
[NH2:13][c:14]1[cH:15][cH:16][cH:17][c:18]2[nH:19][cH:20][cH:21][c:22]12.[O:1]=[C:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[c:10]([Cl:11])[cH:12]1>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[c:10]([Cl:11])[cH:12]1)[NH:13][c:14]1[cH:15][cH:16][cH:17][c:18]2[nH:19][cH:20][cH:21][c:22]12
Nc1cccc2[nH]ccc12.O=C=NCc1ccc(Cl)c(Cl)c1
O=C(NCc1ccc(Cl)c(Cl)c1)Nc1cccc2[nH]ccc12
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2[nH]ccc12
[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH2;D1;+0:5]):[c:6].[O;D1;H0:7]=[C;H0;D2;+0:8]=[N;H0;D2;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:8](=[O;D1;H0:7])-[NH;D2;+0:9]-[C:10]-[c:11]):[c:6]
null
[]
null
null
null
null
4-Aminoindole (0.13 g, 1 mmol) in THF (3 mL) was treated with 1,2-dichloro-4-(isocyanatomethyl)benzene (0.22 g, 1.1 mmol) for 3 h at ambient temperature. Hexane was added to the reaction mixture to precipitate 0.25 g of the title compound as a tan solid. mp 201° C.; 1H NMR (300 MHz, DMSO-d6) δ 4.23 (d, 2H), 6.36 (s, 1H...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
null
C1CCOC1
null
null
Nc1cccc2[nH]ccc12.O=C=NCc1ccc(Cl)c(Cl)c1>C1CCOC1>O=C(NCc1ccc(Cl)c(Cl)c1)Nc1cccc2[nH]ccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-494f09c94a034747a59f95e195d1f93c
Nc1cccc2[nH]ccc12.O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl>>O=C=Nc1cccc2[nH]ccc12
NC1=C2C=CNC2=CC=C1.ClC(Cl)(OC(OC(Cl)(Cl)Cl)=O)Cl>>N(=C=O)C1=C2C=CNC2=CC=C1
[NH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[nH:9][cH:10][cH:11][c:12]12.ClC(Cl)(Cl)O[C:2](OC(Cl)(Cl)Cl)=[O:1]>>[O:1]=[C:2]=[N:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[nH:9][cH:10][cH:11][c:12]12
Nc1cccc2[nH]ccc12.O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl
O=C=Nc1cccc2[nH]ccc12
null
null
C1(=CC=CC=C1)C
Miscellaneous
OtherReaction
38334b31448e1d8428e2cb6569eceaecc2305b2359c734a98433aa0746ff9140
a539b8d5e65abe163774733461d6850ba8234d38df1df3c2ccdeef5ce9de389b
c1ccc2[nH]ccc2c1
Cl-C(-Cl)(-Cl)-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-O-C(-Cl)(-Cl)-Cl.[#7;a:3]:[c:4]:[c:5]:[c:6](-[NH2;D1;+0:7]):[c:8]>>[#7;a:3]:[c:4]:[c:5]:[c:6](-[N;H0;D2;+0:7]=[C;H0;D2;+0:1]=[O;D1;H0:2]):[c:8]
187.3
[{"value": 187.3, "product": "N(=C=O)C1=C2C=CNC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Aminoindole (0.5 g, 3.78 mmol) in toluene (50 mL) was treated with triphosgene (0.4 g, 1.35 mmol) and heated at reflux for 5 hours. The reaction mixture was allowed to cool to room temperature and concentrated under reduced pressure. The residue was taken up in diethyl ether, filtered, and the filtrate was concentrat...
10.6084/m9.figshare.5104873.v1
null
Trichloro group.Trichloro group.Carbonic Ester.Primary amine
Isocyanate
null
null
c1ccc2[nH]ccc2c1
HCl
C1(=CC=CC=C1)C
null
null
Nc1cccc2[nH]ccc12.O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl>C1(=CC=CC=C1)C>O=C=Nc1cccc2[nH]ccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5d5461ba09a34288a079fb380b35d5b0
NCc1ccc(C(F)(F)F)cc1.O=C=Nc1cccc2[nH]ccc12>>O=C(NCc1ccc(C(F)(F)F)cc1)Nc1cccc2[nH]ccc12
CCCCCC.N(=C=O)C1=C2C=CNC2=CC=C1.FC(C1=CC=C(CN)C=C1)(F)F>>N1C=CC2=C(C=CC=C12)NC(=O)NCC1=CC=C(C=C1)C(F)(F)F
[NH2:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[cH:13][cH:14]1.[O:1]=[C:2]=[N:15][c:16]1[cH:17][cH:18][cH:19][c:20]2[nH:21][cH:22][cH:23][c:24]12>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[cH:13][cH:14]1)[NH:15][c:16]1[cH:17][cH:18][cH:19][c:20]2[nH:21][cH:22][cH:2...
NCc1ccc(C(F)(F)F)cc1.O=C=Nc1cccc2[nH]ccc12
O=C(NCc1ccc(C(F)(F)F)cc1)Nc1cccc2[nH]ccc12
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2[nH]ccc12
[#7;a:1]:[c:2]:[c:3]:[c:4](-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7]):[c:8].[NH2;D1;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:9]-[C:10]-[c:11]):[c:8]
null
[]
null
null
3
HOUR
The product of Example 80A (0.15 g, 1 mmol) in THF (3 mL) was treated with 4-(trifluoromethyl)benzylamine (0.19 g, 1.1 mmol) at ambient temperature. After stirring for 3 hours, hexane was added to the reaction mixture to precipitate the title compound as a solid. mp 178° C. 1H NMR (300 MHz, DMSO-d6) δ 4.43 (d, 2H), 6.5...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
null
C1CCOC1
null
3
NCc1ccc(C(F)(F)F)cc1.O=C=Nc1cccc2[nH]ccc12>C1CCOC1>O=C(NCc1ccc(C(F)(F)F)cc1)Nc1cccc2[nH]ccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-402b7bfa394a4b7fa357526ecefe2b68
NCc1ccc(OC(F)(F)F)cc1.O=C=Nc1cccc2[nH]ccc12>>O=C(NCc1ccc(OC(F)(F)F)cc1)Nc1cccc2[nH]ccc12
FC(OC1=CC=C(CN)C=C1)(F)F.N(=C=O)C1=C2C=CNC2=CC=C1>>N1C=CC2=C(C=CC=C12)NC(=O)NCC1=CC=C(C=C1)OC(F)(F)F
[NH2:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([O:9][C:10]([F:11])([F:12])[F:13])[cH:14][cH:15]1.[O:1]=[C:2]=[N:16][c:17]1[cH:18][cH:19][cH:20][c:21]2[nH:22][cH:23][cH:24][c:25]12>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([O:9][C:10]([F:11])([F:12])[F:13])[cH:14][cH:15]1)[NH:16][c:17]1[cH:18][cH:19][cH:20][c:21]2[nH:22]...
NCc1ccc(OC(F)(F)F)cc1.O=C=Nc1cccc2[nH]ccc12
O=C(NCc1ccc(OC(F)(F)F)cc1)Nc1cccc2[nH]ccc12
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2[nH]ccc12
[#7;a:1]:[c:2]:[c:3]:[c:4](-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7]):[c:8].[NH2;D1;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:9]-[C:10]-[c:11]):[c:8]
65.8
[{"value": 65.8, "product": "N1C=CC2=C(C=CC=C12)NC(=O)NCC1=CC=C(C=C1)OC(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-(Trifluoromethoxy)benzylamine (0.21 g, 1.1 mmol) and the product of Example 80A (0.16 g, 1 mmol) were treated as described in Example 80B to provide the title compound (0.23 g). mp 177° C.; 1H NMR (300 MHz, DMSO-d6) δ 4.36 (d, 2H), 6.52 (m, 1H), 6.95 (m, 3H), 7.24 (t, 1H), 7.36 (d, 2H), 7.48 (d, 2H), 7.63 (dd, 1H), 8...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
null
null
null
null
NCc1ccc(OC(F)(F)F)cc1.O=C=Nc1cccc2[nH]ccc12>>O=C(NCc1ccc(OC(F)(F)F)cc1)Nc1cccc2[nH]ccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5e762148a3b14b59a7a4bdab88a889fc
NCc1ccc(C(F)(F)F)c(F)c1.O=C=Nc1cccc2[nH]ccc12>>O=C(NCc1ccc(C(F)(F)F)c(F)c1)Nc1cccc2[nH]ccc12
FC=1C=C(CN)C=CC1C(F)(F)F.N(=C=O)C1=C2C=CNC2=CC=C1>>FC=1C=C(CNC(=O)NC2=C3C=CNC3=CC=C2)C=CC1C(F)(F)F
[NH2:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[c:13]([F:14])[cH:15]1.[O:1]=[C:2]=[N:16][c:17]1[cH:18][cH:19][cH:20][c:21]2[nH:22][cH:23][cH:24][c:25]12>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[c:13]([F:14])[cH:15]1)[NH:16][c:17]1[cH:18][cH:19][cH:20][c:21]2[nH:2...
NCc1ccc(C(F)(F)F)c(F)c1.O=C=Nc1cccc2[nH]ccc12
O=C(NCc1ccc(C(F)(F)F)c(F)c1)Nc1cccc2[nH]ccc12
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2[nH]ccc12
[#7;a:1]:[c:2]:[c:3]:[c:4](-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7]):[c:8].[NH2;D1;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:9]-[C:10]-[c:11]):[c:8]
68.3
[{"value": 68.3, "product": "FC=1C=C(CNC(=O)NC2=C3C=CNC3=CC=C2)C=CC1C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
3-Fluoro-4-(trifluoromethyl)benzylamine (0.22 g, 1.1 mmol) and the product of Example 80A (0.16 g, 1 mmol) were treated as described in Example 80B to provide the title compound (0.24 g). mp 198° C.; 1H NMR (300 MHz, DMSO-d6) δ 4.43 (d, 2H), 6.52 (m, 1H), 6.98 (m, 3H), 7.26 (m, 1H), 7.39 (m, 2H), 7.57 (dd, 1H), 7.77 (t...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
null
null
null
null
NCc1ccc(C(F)(F)F)c(F)c1.O=C=Nc1cccc2[nH]ccc12>>O=C(NCc1ccc(C(F)(F)F)c(F)c1)Nc1cccc2[nH]ccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-27e36248124042f48c694f29083cf12b
NCc1ccc(Cl)c(C(F)(F)F)c1.O=C=Nc1cccc2[nH]ccc12>>O=C(NCc1ccc(Cl)c(C(F)(F)F)c1)Nc1cccc2[nH]ccc12
ClC1=C(C=C(CN)C=C1)C(F)(F)F.N(=C=O)C1=C2C=CNC2=CC=C1>>ClC1=C(C=C(CNC(=O)NC2=C3C=CNC3=CC=C2)C=C1)C(F)(F)F
[NH2:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[c:10]([C:11]([F:12])([F:13])[F:14])[cH:15]1.[O:1]=[C:2]=[N:16][c:17]1[cH:18][cH:19][cH:20][c:21]2[nH:22][cH:23][cH:24][c:25]12>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[c:10]([C:11]([F:12])([F:13])[F:14])[cH:15]1)[NH:16][c:17]1[cH:18][cH:19][cH:20][c:21]2[nH...
NCc1ccc(Cl)c(C(F)(F)F)c1.O=C=Nc1cccc2[nH]ccc12
O=C(NCc1ccc(Cl)c(C(F)(F)F)c1)Nc1cccc2[nH]ccc12
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2[nH]ccc12
[#7;a:1]:[c:2]:[c:3]:[c:4](-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7]):[c:8].[NH2;D1;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:9]-[C:10]-[c:11]):[c:8]
null
[]
null
null
null
null
4-Chloro-3-(trifluoromethyl)benzylamine (0.27 g, 1.1 mmol) and the product of Example 80A (0.16 g, 1 mmol) were treated as described in Example 80B to provide the title compound. mp 197° C.; 1H NMR (300 MHz, DMSO-d6) δ 4.42 (d, 2H), 6.52 (m, 1H), 6.96 (m, 3H), 7.25 (m, 1H), 7.56 (dd, 1H), 7.67 (dd, 1H), 7.70 (t, 1H), 7...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
null
null
null
null
NCc1ccc(Cl)c(C(F)(F)F)c1.O=C=Nc1cccc2[nH]ccc12>>O=C(NCc1ccc(Cl)c(C(F)(F)F)c1)Nc1cccc2[nH]ccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1d4d3376ae5c496abd9fa1a3e8ebab41
NCCc1ccc(Cl)cc1Cl.O=C=Nc1cccc2[nH]ccc12>>O=C(NCCc1ccc(Cl)cc1Cl)Nc1cccc2[nH]ccc12
ClC1=C(C=CC(=C1)Cl)CCN.N(=C=O)C1=C2C=CNC2=CC=C1>>ClC1=C(C=CC(=C1)Cl)CCNC(=O)NC1=C2C=CNC2=CC=C1
[NH2:3][CH2:4][CH2:5][c:6]1[cH:7][cH:8][c:9]([Cl:10])[cH:11][c:12]1[Cl:13].[O:1]=[C:2]=[N:14][c:15]1[cH:16][cH:17][cH:18][c:19]2[nH:20][cH:21][cH:22][c:23]12>>[O:1]=[C:2]([NH:3][CH2:4][CH2:5][c:6]1[cH:7][cH:8][c:9]([Cl:10])[cH:11][c:12]1[Cl:13])[NH:14][c:15]1[cH:16][cH:17][cH:18][c:19]2[nH:20][cH:21][cH:22][c:23]12
NCCc1ccc(Cl)cc1Cl.O=C=Nc1cccc2[nH]ccc12
O=C(NCCc1ccc(Cl)cc1Cl)Nc1cccc2[nH]ccc12
null
null
null
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCc1ccccc1)Nc1cccc2[nH]ccc12
[#7;a:1]:[c:2]:[c:3]:[c:4](-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7]):[c:8].[C:9]-[C:10]-[NH2;D1;+0:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:11]-[C:10]-[C:9]):[c:8]
null
[]
null
null
null
null
2-(2,4-Dichlorophenyl)ethylamine (0.21 g, 1.1 mmol) and the product of Example 80A (0.16 g, 1. mmol) were treated as described in Example 80B to provide the title compound. mp 170° C.; 1H NMR (300 MHz, DMSO-d6) δ 2.90 (m, 2H), 3.31 (m, 2H), 6.47 (m, 2H), 6.93 (m, 2H), 7.23 (m, 1H), 7.40 (m, 2H), 7.60 (m, 2H), 8.15 (s, ...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
null
null
null
null
NCCc1ccc(Cl)cc1Cl.O=C=Nc1cccc2[nH]ccc12>>O=C(NCCc1ccc(Cl)cc1Cl)Nc1cccc2[nH]ccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ec18f9e730094a60b26101a5f64a6926
O=C=Nc1cccc2[nH]ccc12.OCc1ccc(C(F)(F)F)cc1>>O=C(Nc1cccc2[nH]ccc12)OCc1ccc(C(F)(F)F)cc1
FC(C1=CC=C(C=C1)CO)(F)F.N(=C=O)C1=C2C=CNC2=CC=C1.C(C)N(CC)CC>>N1C=CC2=C(C=CC=C12)NC(OCC1=CC=C(C=C1)C(F)(F)F)=O
[O:1]=[C:2]=[N:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[nH:9][cH:10][cH:11][c:12]12.[OH:13][CH2:14][c:15]1[cH:16][cH:17][c:18]([C:19]([F:20])([F:21])[F:22])[cH:23][cH:24]1>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[nH:9][cH:10][cH:11][c:12]12)[O:13][CH2:14][c:15]1[cH:16][cH:17][c:18]([C:19]([F:20])([F:21])[F:22])[cH:23]...
O=C=Nc1cccc2[nH]ccc12.OCc1ccc(C(F)(F)F)cc1
O=C(Nc1cccc2[nH]ccc12)OCc1ccc(C(F)(F)F)cc1
null
null
C1CCOC1
Protection
OtherReaction
8d2aa5da7fec498749aba98cc9467e8d82c146f343570568bec74a92b10e0ae2
e505c5de73b3f9ad0414c141c59109424d376f26a728bbd154d3edfd03d2f50a
O=C(Nc1cccc2[nH]ccc12)OCc1ccccc1
[#7;a:1]:[c:2]:[c:3]:[c:4](-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7]):[c:8].[OH;D1;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[O;H0;D2;+0:9]-[C:10]-[c:11]):[c:8]
53.8
[{"value": 53.8, "product": "N1C=CC2=C(C=CC=C12)NC(OCC1=CC=C(C=C1)C(F)(F)F)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
[4-(Trifluoromethyl)phenyl]methanol (0.09 g, 0.55 mmol) and the product of Example 80A (0.08 g, 0.5 mmol) in THF (5 mL) were heated at reflux for 16 hours with a catalytic amount of triethylamine. The reaction mixture was concentrated under reduced pressure and the residue was purified by chromatography on silica gel e...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary alcohol
Carbamic ester
null
null
c1ccc2[nH]ccc2c1.c1ccccc1
null
C1CCOC1
null
null
O=C=Nc1cccc2[nH]ccc12.OCc1ccc(C(F)(F)F)cc1>C1CCOC1>O=C(Nc1cccc2[nH]ccc12)OCc1ccc(C(F)(F)F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-25703e41bebf41a49b262861f5add80d
O=C=Nc1cccc2[nH]ccc12.OCc1ccc(OC(F)(F)F)cc1>>O=C(Nc1cccc2[nH]ccc12)OCc1ccc(OC(F)(F)F)cc1
FC(OC1=CC=C(C=C1)CO)(F)F.N(=C=O)C1=C2C=CNC2=CC=C1.C(C)N(CC)CC>>N1C=CC2=C(C=CC=C12)NC(OCC1=CC=C(C=C1)OC(F)(F)F)=O
[O:1]=[C:2]=[N:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[nH:9][cH:10][cH:11][c:12]12.[OH:13][CH2:14][c:15]1[cH:16][cH:17][c:18]([O:19][C:20]([F:21])([F:22])[F:23])[cH:24][cH:25]1>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][cH:7][c:8]2[nH:9][cH:10][cH:11][c:12]12)[O:13][CH2:14][c:15]1[cH:16][cH:17][c:18]([O:19][C:20]([F:21])([F:22])[F...
O=C=Nc1cccc2[nH]ccc12.OCc1ccc(OC(F)(F)F)cc1
O=C(Nc1cccc2[nH]ccc12)OCc1ccc(OC(F)(F)F)cc1
null
null
C1CCOC1
Protection
OtherReaction
8d2aa5da7fec498749aba98cc9467e8d82c146f343570568bec74a92b10e0ae2
e505c5de73b3f9ad0414c141c59109424d376f26a728bbd154d3edfd03d2f50a
O=C(Nc1cccc2[nH]ccc12)OCc1ccccc1
[#7;a:1]:[c:2]:[c:3]:[c:4](-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=[O;D1;H0:7]):[c:8].[OH;D1;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[O;H0;D2;+0:9]-[C:10]-[c:11]):[c:8]
54.4
[{"value": 54.4, "product": "N1C=CC2=C(C=CC=C12)NC(OCC1=CC=C(C=C1)OC(F)(F)F)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
[4-(Trifluoromethoxy)pheny]methanol (0.13 g, 0.7 mmol) and the product of Example 80A (0.1 g, 0.63 mmol) in THF (5 mL) were heated at reflux for 16 hours with a catalytic amount of triethylamine. The reaction mixture was concentrated under reduced pressure and the residue was triturated with diethyl ether/hexane to pro...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary alcohol
Carbamic ester
null
null
c1ccc2[nH]ccc2c1.c1ccccc1
null
C1CCOC1
null
null
O=C=Nc1cccc2[nH]ccc12.OCc1ccc(OC(F)(F)F)cc1>C1CCOC1>O=C(Nc1cccc2[nH]ccc12)OCc1ccc(OC(F)(F)F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-93c3b299313148d6920bcc1b4881ba30
Cc1[nH]c2cccc(N)c2c1C.O=C=NCc1ccc(Br)cc1>>Cc1[nH]c2cccc(NC(=O)NCc3ccc(Br)cc3)c2c1C
CCCCCC.CC=1NC2=CC=CC(=C2C1C)N.BrC1=CC=C(C=C1)CN=C=O>>BrC1=CC=C(CNC(=O)NC2=C3C(=C(NC3=CC=C2)C)C)C=C1
[CH3:1][c:2]1[nH:3][c:4]2[cH:5][cH:6][cH:7][c:8]([NH2:9])[c:21]2[c:22]1[CH3:23].[C:10](=[O:11])=[N:12][CH2:13][c:14]1[cH:15][cH:16][c:17]([Br:18])[cH:19][cH:20]1>>[CH3:1][c:2]1[nH:3][c:4]2[cH:5][cH:6][cH:7][c:8]([NH:9][C:10](=[O:11])[NH:12][CH2:13][c:14]3[cH:15][cH:16][c:17]([Br:18])[cH:19][cH:20]3)[c:21]2[c:22]1[CH3:2...
Cc1[nH]c2cccc(N)c2c1C.O=C=NCc1ccc(Br)cc1
Cc1[nH]c2cccc(NC(=O)NCc3ccc(Br)cc3)c2c1C
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2[nH]ccc12
[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH2;D1;+0:5]):[c:6].[O;D1;H0:7]=[C;H0;D2;+0:8]=[N;H0;D2;+0:9]-[C:10]-[c:11]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[NH;D2;+0:5]-[C;H0;D3;+0:8](=[O;D1;H0:7])-[NH;D2;+0:9]-[C:10]-[c:11]):[c:6]
null
[]
null
null
3
HOUR
2,3-Dimethyl-4-aminoindole (0.11 g, 0.7 mmol) in THF (3 mL) was treated with 1-bromo-4-(isocyanatomethyl)benzene (0.17 g, 0.8 mmol) at ambient temperature. After stirring for 3 hours at ambient temperature, hexane was added to the reaction mixture to precipitate the title compound as a tan solid (0.12 g). mp 190° C. 1H...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccc2[nH]ccc2c1.c1ccccc1
null
C1CCOC1
null
3
Cc1[nH]c2cccc(N)c2c1C.O=C=NCc1ccc(Br)cc1>C1CCOC1>Cc1[nH]c2cccc(NC(=O)NCc3ccc(Br)cc3)c2c1C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2f3cfefeb8ee42058587f4c73297002d
O=[N+]([O-])c1cccc2[nH]ncc12>>Nc1cccc2[nH]ncc12
[BH4-].[Na+].[N+](=O)([O-])C1=C2C=NNC2=CC=C1>>N1N=CC=2C(=CC=CC12)N
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][cH:5][c:6]2[nH:7][n:8][cH:9][c:10]12>>[NH2:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[nH:7][n:8][cH:9][c:10]12
O=[N+]([O-])c1cccc2[nH]ncc12
Nc1cccc2[nH]ncc12
null
null
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2[nH]ncc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]1:[c:5]:[#7;a:6]:[#7;a:7]:[c:8]:1>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]1:[c:5]:[#7;a:6]:[#7;a:7]:[c:8]:1
75.1
[{"value": 75.1, "product": "N1N=CC=2C(=CC=CC12)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
4-Nitro-1H-indazole (1.63 g, 10 mmol) in ethanol (100 mL) was treated with BiCl3 (3.46 g, 11 mmol) followed by a portionwise addition of NaBH4. The reaction mixture was stirred at ambient temperature for 20 minutes and filtered through Celite. The filtrate was evaporated under reduced pressure and the residue was parti...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2[nH]ncc2c1
Other
C(C)O
null
0.333333
O=[N+]([O-])c1cccc2[nH]ncc12>C(C)O>Nc1cccc2[nH]ncc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d1cd8c040b014a86b3af0bab367a7a2d
COC(=O)Cl.O=[N+]([O-])c1cccc2[nH]ncc12>>COC(=O)n1ncc2c([N+](=O)[O-])cccc21
O.[H-].[Na+].[N+](=O)([O-])C1=C2C=NNC2=CC=C1.COC(=O)Cl>>[N+](=O)([O-])C1=C2C=NN(C2=CC=C1)C(=O)OC
Cl[C:3]([O:2][CH3:1])=[O:4].[nH:5]1[n:6][cH:7][c:8]2[c:9]([N+:10](=[O:11])[O-:12])[cH:13][cH:14][cH:15][c:16]12>>[CH3:1][O:2][C:3](=[O:4])[n:5]1[n:6][cH:7][c:8]2[c:9]([N+:10](=[O:11])[O-:12])[cH:13][cH:14][cH:15][c:16]12
COC(=O)Cl.O=[N+]([O-])c1cccc2[nH]ncc12
COC(=O)n1ncc2c([N+](=O)[O-])cccc21
null
null
CN(C)C=O
Acylation
N-alkylation of secondary amines with alkyl halides
7faa17e35f4b23d2a80e9918e1703cff18db9438f8afa208f5b9468b7244c1c3
d03c43b1eb3e007d0a26c663cd0f6b51f594c27d1ade9616fb1640d35a60bddb
c1ccc2[nH]ncc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4].[c:5]:[c:6]1:[c:7]:[c:8]:[#7;a:9]:[nH;D2;+0:10]:1>>[C;D1;H3:4]-[#8:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[n;H0;D3;+0:10]1:[#7;a:9]:[c:8]:[c:7]:[c:6]:1:[c:5]
null
[]
null
null
1
HOUR
Sodium hydride (0.3 g, 12.5 mmol) suspended in DMF (5 mL) at 0° C. was treated with 4-nitro-1H-indazole (1.33 g, 10 mmol). After stirring at room temperature for 1 hours, the mixture was treated with methylchloroformate (0.9 mL). After stirring at room temperature for 3 hours, the mixture was carefully treated with wat...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether
Ether
c1ccc2[nH]ncc2c1
c1cccc2[nH]ncc12
c1cccc2[nH]ncc12
HCl
CN(C)C=O
null
1
COC(=O)Cl.O=[N+]([O-])c1cccc2[nH]ncc12>CN(C)C=O>COC(=O)n1ncc2c([N+](=O)[O-])cccc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-76f351b7aaeb48c2a08b8b641d36c13e
COC(=O)n1ncc2c([N+](=O)[O-])cccc21>>COC(=O)n1ncc2c(N)cccc21
[BH4-].[Na+].[N+](=O)([O-])C1=C2C=NN(C2=CC=C1)C(=O)OC>>NC1=C2C=NN(C2=CC=C1)C(=O)OC
O=[N+:10]([O-])[c:9]1[c:8]2[cH:7][n:6][n:5]([C:3]([O:2][CH3:1])=[O:4])[c:14]2[cH:13][cH:12][cH:11]1>>[CH3:1][O:2][C:3](=[O:4])[n:5]1[n:6][cH:7][c:8]2[c:9]([NH2:10])[cH:11][cH:12][cH:13][c:14]12
COC(=O)n1ncc2c([N+](=O)[O-])cccc21
COC(=O)n1ncc2c(N)cccc21
null
null
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2[nH]ncc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]1:[c:5]:[#7;a:6]:[#7;a:7]:[c:8]:1>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]1:[c:5]:[#7;a:6]:[#7;a:7]:[c:8]:1
83.7
[{"value": 83.7, "product": "NC1=C2C=NN(C2=CC=C1)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
The product of Example 90A (1.66 g, 7.5 mmol) in ethanol (20 mL) was treated with BiCl3 (8.2 g, 2.6 mmol) followed by the addition of NaBH4 (1.13 g, 30.5 mmol). The reaction mixture was stirred at room temperature for 20 minutes, filtered through Celite, and the filtrate was evaporated under reduced pressure. The resid...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1cccc2[nH]ncc12
Other
C(C)O
null
0.333333
COC(=O)n1ncc2c([N+](=O)[O-])cccc21>C(C)O>COC(=O)n1ncc2c(N)cccc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0799dee62d2d45c1bc621be2a0256ced
COC(=O)n1ncc2c(N)cccc21.O=C=NCc1ccc(Cl)c(Cl)c1>>COC(=O)n1ncc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc21
CCCCCC.NC1=C2C=NN(C2=CC=C1)C(=O)OC.ClC1=C(C=C(C=C1)CN=C=O)Cl>>ClC=1C=C(CNC(=O)NC2=C3C=NN(C3=CC=C2)C(=O)OC)C=CC1Cl
[CH3:1][O:2][C:3](=[O:4])[n:5]1[n:6][cH:7][c:8]2[c:9]([NH2:10])[cH:23][cH:24][cH:25][c:26]12.[C:11](=[O:12])=[N:13][CH2:14][c:15]1[cH:16][cH:17][c:18]([Cl:19])[c:20]([Cl:21])[cH:22]1>>[CH3:1][O:2][C:3](=[O:4])[n:5]1[n:6][cH:7][c:8]2[c:9]([NH:10][C:11](=[O:12])[NH:13][CH2:14][c:15]3[cH:16][cH:17][c:18]([Cl:19])[c:20]([C...
COC(=O)n1ncc2c(N)cccc21.O=C=NCc1ccc(Cl)c(Cl)c1
COC(=O)n1ncc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc21
null
null
C1CCOC1
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCc1ccccc1)Nc1cccc2[nH]ncc12
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]1:[c:5]:[#7;a:6]:[#7;a:7]:[c:8]:1.[O;D1;H0:9]=[C;H0;D2;+0:10]=[N;H0;D2;+0:11]-[C:12]-[c:13]>>[O;D1;H0:9]=[C;H0;D3;+0:10](-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]1:[c:5]:[#7;a:6]:[#7;a:7]:[c:8]:1)-[NH;D2;+0:11]-[C:12]-[c:13]
null
[]
null
null
3
HOUR
The product of Example 90B (0.19 g, 1 mmol) in THF (3 mL) was treated with 1,2-dichloro-4-(isocyanatomethyl)benzene (0.22 g, 1.1 mmol) at ambient temperature. After stirring for 3 hours, hexane was added to the reaction mixture to precipitate the title compound as a tan solid (0.25 g). 1H NMR (300 MHz, DMSO-d6) δ 4.38 ...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccccc1.c1cccc2[nH]ncc12
null
C1CCOC1
null
3
COC(=O)n1ncc2c(N)cccc21.O=C=NCc1ccc(Cl)c(Cl)c1>C1CCOC1>COC(=O)n1ncc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e811c5f2db5a4baba03798fd855c4f85
COC(=O)n1ncc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc21>>O=C(NCc1ccc(Cl)c(Cl)c1)Nc1cccc2[nH]ncc12
ClC=1C=C(CNC(=O)NC2=C3C=NN(C3=CC=C2)C(=O)OC)C=CC1Cl.[OH-].[K+].C(Cl)Cl.O>>ClC=1C=C(CNC(=O)NC2=C3C=NNC3=CC=C2)C=CC1Cl
COC(=O)[n:19]1[c:18]2[cH:17][cH:16][cH:15][c:14]([NH:13][C:2](=[O:1])[NH:3][CH2:4][c:5]3[cH:6][cH:7][c:8]([Cl:9])[c:10]([Cl:11])[cH:12]3)[c:22]2[cH:21][n:20]1>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[c:10]([Cl:11])[cH:12]1)[NH:13][c:14]1[cH:15][cH:16][cH:17][c:18]2[nH:19][n:20][cH:21][c:22]12
COC(=O)n1ncc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc21
O=C(NCc1ccc(Cl)c(Cl)c1)Nc1cccc2[nH]ncc12
null
null
CO
Reduction
OtherReaction
b2164736883446cc727e745d0b4fddbc945c5a6fa5cfea478691c70222eeb795
84394d34c591024a84d9393eb3e8adb8ada5a6225c3abafc4dae9aedd4568be4
O=C(NCc1ccccc1)Nc1cccc2[nH]ncc12
C-O-C(=O)-[n;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c:5]:1:[c:6]>>[c:6]:[c:5]1:[c:4]:[c:3]:[#7;a:2]:[nH;D2;+0:1]:1
null
[]
null
null
null
null
The product of Example 90C (0.25 g, 0.6 mmol) was heated at reflux in methanol (5 mL) and 0.5N KOH (1 mL) for 0.5 hours. The reaction mixture was allowed to cool to ambient temperature, pH was adjusted to 5, and volume was reduced under reduced pressure. Methylene chloride and water was added, the phases were separated...
10.6084/m9.figshare.5104873.v1
null
Ether
null
c1cccc2[nH]ncc12
c1ccc2[nH]ncc2c1
c1ccccc1.c1ccc2[nH]ncc2c1
HO-
CO
null
null
COC(=O)n1ncc2c(NC(=O)NCc3ccc(Cl)c(Cl)c3)cccc21>CO>O=C(NCc1ccc(Cl)c(Cl)c1)Nc1cccc2[nH]ncc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-28b7ce7cf2a34f658965fc61001c81c1
C=C(C)CC(O)(C(=O)OCC)C(F)(F)F.COc1ccc(F)cc1>>CCOC(=O)C(O)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F
C(C)OC(C(CC(=C)C)(C(F)(F)F)O)=O.FC1=CC=C(C=C1)OC.[Cl-].[Al+3].[Cl-].[Cl-]>>C(C)OC(C(CC(C)(C)C1=C(C=CC(=C1)F)OC)(C(F)(F)F)O)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([OH:7])([CH2:8][C:9]([CH3:10])=[CH2:11])[C:21]([F:22])([F:23])[F:24].[cH:12]1[cH:13][c:14]([F:15])[cH:16][cH:17][c:18]1[O:19][CH3:20]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([OH:7])([CH2:8][C:9]([CH3:10])([CH3:11])[c:12]1[cH:13][c:14]([F:15])[cH:16][cH:17][c:18]1[O:19][CH3:20])[C:21...
C=C(C)CC(O)(C(=O)OCC)C(F)(F)F.COc1ccc(F)cc1
CCOC(=O)C(O)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F
null
null
null
C-C Coupling
Friedel-Crafts alkylation
f6021e53f57d07d48a856391b21137517c9bd669381174a55381b6219a6afd68
48297e5b607b4624d5b08506879ba8f9dd47fb272c10888542fa01ef83829ef2
c1ccccc1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[C;H0;D3;+0:6](-[C;D1;H3:7])=[CH2;D1;+0:8].[#8:9]-[c:10](:[c:11]):[cH;D2;+0:12]:[c:13]:[c:14]>>[#8:9]-[c:10](:[c:11]):[c;H0;D3;+0:12](-[C;H0;D4;+0:6](-[C;D1;H3:7])(-[CH3;D1;+0:8])-[C:5]-[C:4]-[C:2](-[#8:1])=[O;D1;H0:3]):[c:13]:[c:14]
71
[{"value": 71.0, "product": "C(C)OC(C(CC(C)(C)C1=C(C=CC(=C1)F)OC)(C(F)(F)F)O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3
DAY
To a mixture of 5.9 g (26.1 mmol) of the above 2-hydroxy-4-methyl-2-trifluoromethylpent-4-enoic acid ethyl ester in 30 mL of 4-fluoroanisole was added 5.2 g (39.4 mmol) of aluminum chloride in several portions. The mixture became exothermic and turned black with the first addition and was cooled with an ice-water bath....
10.6084/m9.figshare.5104873.v1
null
Vinyl
null
c1ccccc1
c1ccccc1
c1ccccc1
null
null
null
72
C=C(C)CC(O)(C(=O)OCC)C(F)(F)F.COc1ccc(F)cc1>>CCOC(=O)C(O)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0f255b62e0074ac9bcc1cd1bc6738ed5
CCOC(=O)C(O)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F>>COc1ccc(F)cc1C(C)(C)CC(O)(CO)C(F)(F)F
C(C)OC(C(CC(C)(C)C1=C(C=CC(=C1)F)OC)(C(F)(F)F)O)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>FC=1C=CC(=C(C1)C(CC(CO)(O)C(F)(F)F)(C)C)OC
CCO[C:16]([C:14]([CH2:13][C:10]([c:9]1[c:3]([O:2][CH3:1])[cH:4][cH:5][c:6]([F:7])[cH:8]1)([CH3:11])[CH3:12])([OH:15])[C:18]([F:19])([F:20])[F:21])=[O:17]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3:12])[CH2:13][C:14]([OH:15])([CH2:16][OH:17])[C:18]([F:19])([F:20])[F:21]
CCOC(=O)C(O)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F
COc1ccc(F)cc1C(C)(C)CC(O)(CO)C(F)(F)F
null
null
C1CCOC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccccc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3](-[C:4])(-[O;D1;H1:5])-[C:6](-[F;D1;H0:7])(-[F;D1;H0:8])-[F;D1;H0:9]>>[C:4]-[C:3](-[O;D1;H1:5])(-[CH2;D2;+0:1]-[OH;D1;+0:2])-[C:6](-[F;D1;H0:7])(-[F;D1;H0:8])-[F;D1;H0:9]
92.9
[{"value": 92.0, "product": "FC=1C=CC(=C(C1)C(CC(CO)(O)C(F)(F)F)(C)C)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.9, "product": "FC=1C=CC(=C(C1)C(CC(CO)(O)C(F)(F)F)(C)C)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a chilled solution (ice-water bath) of 6 g (17.0 mmol) of the above 4-(5-fluoro-2-methoxyphenyl)-2-hydroxy-4-methyl-2-trifluoromethylpentanoic acid ethyl ester in 60 mL of dry THF, 2.4 g (61.5 mmol) of lithium aluminum hydride was added in portions. After the addition, the cold bath was removed and the mixture was s...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccccc1
HO-
C1CCOC1
null
8
CCOC(=O)C(O)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F>C1CCOC1>COc1ccc(F)cc1C(C)(C)CC(O)(CO)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b41be51826db4d2eb77745541df9b0f1
COc1ccc(F)cc1C(C)(C)CC(O)(CO)C(F)(F)F>>COc1ccc(F)cc1C(C)(C)CC(=O)C(F)(F)F
FC=1C=CC(=C(C1)C(CC(CO)(O)C(F)(F)F)(C)C)OC.I(=O)(=O)(=O)[O-].[Na+]>>FC(C(CC(C)(C)C1=C(C=CC(=C1)F)OC)=O)(F)F
OC[C:14]([CH2:13][C:10]([c:9]1[c:3]([O:2][CH3:1])[cH:4][cH:5][c:6]([F:7])[cH:8]1)([CH3:11])[CH3:12])([OH:15])[C:16]([F:17])([F:18])[F:19]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3:12])[CH2:13][C:14](=[O:15])[C:16]([F:17])([F:18])[F:19]
COc1ccc(F)cc1C(C)(C)CC(O)(CO)C(F)(F)F
COc1ccc(F)cc1C(C)(C)CC(=O)C(F)(F)F
null
null
CCCCCC.CCOCC.CO
Miscellaneous
OtherReaction
81a20ed57ee1ee8b55e4a533e6a354ed57ac5ba5659b8e1dd3b74910e43debde
d8333db1a8553533b9f31a51fd46ac10421b6606be90ce648ca3b16dc0428896
c1ccccc1
O-C-[C;H0;D4;+0:1](-[OH;D1;+0:2])(-[C:3]-[C:4])-[C:5](-[F;D1;H0:6])(-[F;D1;H0:7])-[F;D1;H0:8]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:5](-[F;D1;H0:6])(-[F;D1;H0:7])-[F;D1;H0:8]
87.6
[{"value": 87.0, "product": "FC(C(CC(C)(C)C1=C(C=CC(=C1)F)OC)=O)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.6, "product": "FC(C(CC(C)(C)C1=C(C=CC(=C1)F)OC)=O)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
To a solution of 4.9 g (15.8 mmol) of the above 4-(5-fluoro-2-methoxyphenyl)-4-methyl-2-trifluoromethylpentane-1,2-diol in 100 mL of MeOH was added 10 g (45.9 mmol) of sodium periodate. The mixture was stirred for 4 hours and was then diluted with 100 mL of ether and 100 mL of hexane, filtered through diatomaceous eart...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Tertiary alcohol
Ketone
null
null
c1ccccc1
HO-
CCCCCC.CCOCC.CO
null
4
COc1ccc(F)cc1C(C)(C)CC(O)(CO)C(F)(F)F>CCCCCC.CCOCC.CO>COc1ccc(F)cc1C(C)(C)CC(=O)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c5aea3bb6c7145c0a83278b7a1d1572c
CC(C)(C)S(N)=O.COc1ccc(F)cc1C(C)(C)CC(=O)C(F)(F)F>>COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F
FC(C(CC(C)(C)C1=C(C=CC(=C1)F)OC)=O)(F)F.C(C)(C)(C)S(=O)N>>FC=1C=CC(=C(C1)C(C/C(/C(F)(F)F)=N/S(=O)C(C)(C)C)(C)C)OC
[NH2:15][S:16](=[O:17])[C:18]([CH3:19])([CH3:20])[CH3:21].O=[C:14]([CH2:13][C:10]([c:9]1[c:3]([O:2][CH3:1])[cH:4][cH:5][c:6]([F:7])[cH:8]1)([CH3:11])[CH3:12])[C:22]([F:23])([F:24])[F:25]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3:12])[CH2:13]/[C:14](=[N:15]/[S:16](=[O:17])[C:18]([CH3:1...
CC(C)(C)S(N)=O.COc1ccc(F)cc1C(C)(C)CC(=O)C(F)(F)F
COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F
null
null
[Cl-].[Na+].O.CCO.CCOC(=O)C.C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
c1ccccc1
O=[C;H0;D3;+0:1](-[C:2]-[C:3])-[C:4](-[F;D1;H0:5])(-[F;D1;H0:6])-[F;D1;H0:7].[C:8]-[#16:9](-[NH2;D1;+0:10])=[O;D1;H0:11]>>[C:3]-[C:2]/[C;H0;D3;+0:1](=[N;H0;D2;+0:10]/[#16:9](-[C:8])=[O;D1;H0:11])-[C:4](-[F;D1;H0:5])(-[F;D1;H0:6])-[F;D1;H0:7]
44
[{"value": 44.0, "product": "FC=1C=CC(=C(C1)C(C/C(/C(F)(F)F)=N/S(=O)C(C)(C)C)(C)C)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 43.7, "product": "FC=1C=CC(=C(C1)C(C/C(/C(F)(F)F)=N/S(=O)C(C)(C)C)(C)C)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a mixture of 500 mg (1.8 mmol) of 1,1,1-trifluoro-4-(5-fluoro-2-methoxyphenyl)-4-methylpentan-2-one and 0.86 mL (3.6 mmol) of a solution of Ti(OEt)4 in EtOH (˜20% Ti) in 7 mL of THF was added 240 mg (2 mmol) t-butylsulfinamide. The reaction was warmed at reflux for 6 h and then cooled to room temperature, diluted wi...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1
HO-
[Cl-].[Na+].O.CCO.CCOC(=O)C.C1CCOC1
null
null
CC(C)(C)S(N)=O.COc1ccc(F)cc1C(C)(C)CC(=O)C(F)(F)F>[Cl-].[Na+].O.CCO.CCOC(=O)C.C1CCOC1>COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ad8536782cee4311a9561ad7db6d3bb1
CC(C)([CH2][Mg][Cl])c1ccccc1.CCOC(=O)C(=O)C(F)(F)F>>CCOC(=O)C(O)(CC(C)(C)c1ccccc1)C(F)(F)F
CC(C[Mg]Cl)(C)C1=CC=CC=C1.FC(C(C(=O)OCC)=O)(F)F>>C(C)OC(C(CC(C)(C1=CC=CC=C1)C)(C(F)(F)F)O)=O
[Cl][Mg][CH2:8][C:9]([CH3:10])([CH3:11])[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](=[O:7])[C:18]([F:19])([F:20])[F:21]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([OH:7])([CH2:8][C:9]([CH3:10])([CH3:11])[c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1)[C:18]([F:19])([F:20])[F:21]
CC(C)([CH2][Mg][Cl])c1ccccc1.CCOC(=O)C(=O)C(F)(F)F
CCOC(=O)C(O)(CC(C)(C)c1ccccc1)C(F)(F)F
null
null
C(C)OCC.C1CCOC1
C-C Coupling
Grignard from ketone to alcohol
c19641c06a40b22fede7d393a1da1cf27beb2cebc8cc85022080aa1ae052c9db
652461eb0cd30990fcbed359f728e518ea93a58c037f4fc210fcb30d2dae5f8d
c1ccccc1
[C;D1;H3:1]-[C:2](-[C;D1;H3:3])(-[c:4])-[CH2;D2;+0:5]-[Mg]-[Cl].[C:6]-[#8:7]-[C:8](=[O;D1;H0:9])-[C;H0;D3;+0:10](=[O;H0;D1;+0:11])-[C:12](-[F;D1;H0:13])(-[F;D1;H0:14])-[F;D1;H0:15]>>[C:6]-[#8:7]-[C:8](=[O;D1;H0:9])-[C;H0;D4;+0:10](-[OH;D1;+0:11])(-[CH2;D2;+0:5]-[C:2](-[C;D1;H3:1])(-[C;D1;H3:3])-[c:4])-[C:12](-[F;D1;H0:...
67
[{"value": 67.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a room temperature solution of 45 mL (22.5 mmol) of a 0.5 M solution of 2-methyl-2-phenylpropylmagnesium chloride in diethyl ether was added 38 g (22.5 mmol) of ethyl trifluoropyruvate in 10 mL of anhydrous THF. The reaction became slightly warm to the touch and a white precipitate quickly developed. After 2 hours, ...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Ketone.Ester
Ester.Tertiary alcohol
null
null
c1ccccc1
Mg
C(C)OCC.C1CCOC1
null
2
CC(C)([CH2][Mg][Cl])c1ccccc1.CCOC(=O)C(=O)C(F)(F)F>C(C)OCC.C1CCOC1>CCOC(=O)C(O)(CC(C)(C)c1ccccc1)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1f92c4dbb5644799998fc794518485ad
CC(C)=CC(=O)C(F)(F)F.Fc1cc[c]([Mg][Br])cc1>>CC(C)(CC(=O)C(F)(F)F)c1ccc(F)cc1
CCOCC.C1CCOC1.FC(C(C=C(C)C)=O)(F)F.FC1=CC=C(C=C1)[Mg]Br>>FC(C(CC(C)(C)C1=CC=C(C=C1)F)=O)(F)F
[CH3:1][C:2]([CH3:3])=[CH:4][C:5](=[O:6])[C:7]([F:8])([F:9])[F:10].[Br][Mg][c:11]1[cH:12][cH:13][c:14]([F:15])[cH:16][cH:17]1>>[CH3:1][C:2]([CH3:3])([CH2:4][C:5](=[O:6])[C:7]([F:8])([F:9])[F:10])[c:11]1[cH:12][cH:13][c:14]([F:15])[cH:16][cH:17]1
CC(C)=CC(=O)C(F)(F)F.Fc1cc[c]([Mg][Br])cc1
CC(C)(CC(=O)C(F)(F)F)c1ccc(F)cc1
null
[Cu]I
CCOCC
C-C Coupling
OtherReaction
acaaa339865910ee0f39da9928705a9efb5b9d834fb78bc685b81a374a75bca3
135f2ea95ad9a9b731f59e3aadf4d42e0f9aa41135665e9340592661a7692c1c
c1ccccc1
[Br]-[Mg]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[C;D1;H3:6]-[C;H0;D3;+0:7](-[C;D1;H3:8])=[CH;D2;+0:9]-[C:10](=[O;D1;H0:11])-[C:12](-[F;D1;H0:13])(-[F;D1;H0:14])-[F;D1;H0:15]>>[C;D1;H3:6]-[C;H0;D4;+0:7](-[C;D1;H3:8])(-[CH2;D2;+0:9]-[C:10](=[O;D1;H0:11])-[C:12](-[F;D1;H0:13])(-[F;D1;H0:14])-[F;D1;H0:15])-[c;H0;D3;+0:1...
null
[]
null
null
2
HOUR
To a 2 M ether/THF solution of the above 1,1,1-trifluoro-4-methylpent-3-en-2-one was added 3.8 g of CuI and 10 mL of 2 M ether solution of 4-fluorophenylmagnesium bromide at 0° C. The mixture was warmed to room temperature and stirred for 2 hours. The reaction was quenched with saturated aqueous ammonium chloride and e...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Ketone
Ketone
c1ccccc1
c1ccccc1
c1ccccc1
Br-.Mg
[Cu]I.CCOCC
null
2
CC(C)=CC(=O)C(F)(F)F.Fc1cc[c]([Mg][Br])cc1>[Cu]I.CCOCC>CC(C)(CC(=O)C(F)(F)F)c1ccc(F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0f6a1e981b314c1c9c77fdfca8695d2a
COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F.Cc1ccccn1>>COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccccn1)C(F)(F)F
FC=1C=CC(=C(C1)C(C/C(/C(F)(F)F)=N/S(=O)C(C)(C)C)(C)C)OC.[Li]C(C)(C)C.CC1=NC=CC=C1>>FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=NC=CC=C1)N)(C)C)OC
CC(C)(C)S(=O)/[N:15]=[C:14](/[CH2:13][C:10]([c:9]1[c:3]([O:2][CH3:1])[cH:4][cH:5][c:6]([F:7])[cH:8]1)([CH3:11])[CH3:12])[C:23]([F:24])([F:25])[F:26].[CH3:16][c:17]1[cH:18][cH:19][cH:20][cH:21][n:22]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3:12])[CH2:13][C:14]([NH2:15])([CH2:16][c:17]...
COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F.Cc1ccccn1
COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccccn1)C(F)(F)F
null
null
CCCCC.C1CCOC1
C-C Coupling
OtherReaction
ea3670267116d5783ab698a14a0529569267399ee692198612de216b6780a4f2
a891e3efbb7d17d9024318bc2cb873f9c84846ffdaa21e6d4dd6f86dbec3bf20
c1ccc(CCCCc2ccccn2)cc1
C-C(-C)(-C)-S(=O)/[N;H0;D2;+0:1]=[C;H0;D3;+0:2](/[C:3]-[C:4])-[C:5](-[F;D1;H0:6])(-[F;D1;H0:7])-[F;D1;H0:8].[CH3;D1;+0:9]-[c:10](:[c:11]):[#7;a:12]:[c:13]>>[C:4]-[C:3]-[C;H0;D4;+0:2](-[NH2;D1;+0:1])(-[CH2;D2;+0:9]-[c:10](:[c:11]):[#7;a:12]:[c:13])-[C:5](-[F;D1;H0:6])(-[F;D1;H0:7])-[F;D1;H0:8]
25.2
[{"value": 25.0, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=NC=CC=C1)N)(C)C)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 25.2, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=NC=CC=C1)N)(C)C)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a chilled (−78 C.) solution of 0.05 mL (0.514 mmol) of 2-methylpyridine in 3 mL of dry THF was added 0.23 mL (0.4 mmol) of a 1.7 M solution of t-BuLi in pentane. The mixture turned a bright orange. After 10 min, a solution of 98 mg (0.257 mmol) of 2-methyl-propane-2-sulfinic acid [3-(5-fluoro-2-methoxy-phenyl)-3-met...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
null
null
c1ccccc1.c1ccncc1
Other
CCCCC.C1CCOC1
null
0.166667
COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F.Cc1ccccn1>CCCCC.C1CCOC1>COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccccn1)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dbe22f1cc4b247bc8ad311fec8f58b7a
COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F.Cc1cc2ccccc2[nH]1>>COc1ccc(F)cc1C(C)(C)CC(N)(Cc1cc2ccccc2[nH]1)C(F)(F)F
FC=1C=CC(=C(C1)C(C/C(/C(F)(F)F)=N/S(=O)C(C)(C)C)(C)C)OC.CC(C)(C)[O-].[K+].[Li]CCCC.CC=1NC2=CC=CC=C2C1>>FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC=1NC2=CC=CC=C2C1)N)(C)C)OC
CC(C)(C)S(=O)/[N:15]=[C:14](/[CH2:13][C:10]([c:9]1[c:3]([O:2][CH3:1])[cH:4][cH:5][c:6]([F:7])[cH:8]1)([CH3:11])[CH3:12])[C:26]([F:27])([F:28])[F:29].[CH3:16][c:17]1[cH:18][c:19]2[cH:20][cH:21][cH:22][cH:23][c:24]2[nH:25]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3:12])[CH2:13][C:14]([N...
COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F.Cc1cc2ccccc2[nH]1
COc1ccc(F)cc1C(C)(C)CC(N)(Cc1cc2ccccc2[nH]1)C(F)(F)F
null
null
C(C)OCC.C1CCOC1
C-C Coupling
OtherReaction
ea3670267116d5783ab698a14a0529569267399ee692198612de216b6780a4f2
a891e3efbb7d17d9024318bc2cb873f9c84846ffdaa21e6d4dd6f86dbec3bf20
c1ccc(CCCCc2cc3ccccc3[nH]2)cc1
C-C(-C)(-C)-S(=O)/[N;H0;D2;+0:1]=[C;H0;D3;+0:2](/[C:3]-[C:4])-[C:5](-[F;D1;H0:6])(-[F;D1;H0:7])-[F;D1;H0:8].[CH3;D1;+0:9]-[c:10](:[c:11]):[#7;a:12]:[c:13]>>[C:4]-[C:3]-[C;H0;D4;+0:2](-[NH2;D1;+0:1])(-[CH2;D2;+0:9]-[c:10](:[c:11]):[#7;a:12]:[c:13])-[C:5](-[F;D1;H0:6])(-[F;D1;H0:7])-[F;D1;H0:8]
33
[{"value": 33.0, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC=1NC2=CC=CC=C2C1)N)(C)C)OC", "details": "PERCENTYIELD", "is_desired": false}]
-78
CELSIUS
5
MINUTE
To a chilled (−78 C.) solution of 40 mg (0.30 mmol) of 2-methylindole in 3 mL of diethyl ether was added 0.56 mL (0.91 mmol) of a 1.6 M solution of n-BuLi in hexanes. The resulting orange solution was stirred for 5 min and treated with 0.60 mL (0.60 mmol) of a solution of 1 M solution of KOt-Bu in THF. The reaction was...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
null
null
c1ccccc1.c1ccc2[nH]ccc2c1
Other
C(C)OCC.C1CCOC1
-78
0.083333
COc1ccc(F)cc1C(C)(C)C/C(=N/S(=O)C(C)(C)C)C(F)(F)F.Cc1cc2ccccc2[nH]1>C(C)OCC.C1CCOC1>COc1ccc(F)cc1C(C)(C)CC(N)(Cc1cc2ccccc2[nH]1)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-78f61fc663da4dc2a337552f1b74b830
C=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F>>CNC(Cc1ccnc2ccccc12)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F
C(C)(=O)O.C(C)(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+].FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)N)(C)C)OC.C=O>>FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)NC)(C)C)OC
O=[CH2:1].[NH2:2][C:3]([CH2:4][c:5]1[cH:6][cH:7][n:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]12)([CH2:15][C:16]([CH3:17])([CH3:18])[c:19]1[cH:20][c:21]([F:22])[cH:23][cH:24][c:25]1[O:26][CH3:27])[C:28]([F:29])([F:30])[F:31]>>[CH3:1][NH:2][C:3]([CH2:4][c:5]1[cH:6][cH:7][n:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]12)([C...
C=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F
CNC(Cc1ccnc2ccccc12)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F
null
null
ClC(C)Cl
Heteroatom Alkylation and Arylation
Reductive methylation of primary amine with formaldehyde
51d235def9103cd7a524cbedb590276839772d481304df37a121e64cb81721f4
cf32f1267c674fd84d46b8a676a46bd4e3a018dea282d34ea9ab93d79b66d0ee
c1ccc(CCCCc2ccnc3ccccc23)cc1
O=[CH2;D1;+0:1].[C:2]-[C:3](-[C:4])(-[NH2;D1;+0:5])-[C:6](-[F;D1;H0:7])(-[F;D1;H0:8])-[F;D1;H0:9]>>[C:2]-[C:3](-[C:4])(-[NH;D2;+0:5]-[CH3;D1;+0:1])-[C:6](-[F;D1;H0:7])(-[F;D1;H0:8])-[F;D1;H0:9]
55.2
[{"value": 55.0, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)NC)(C)C)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 55.2, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)NC)(C)C)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
A solution of 3-(5-fluoro-2-methoxy-phenyl)-3-methyl-1-quinolin-4-ylmethyl-1-trifluoromethyl-butylamine (42.0 mg, 0.1 mmol) and formaldehyde (8 μL, 0.1 mmol) in dichloroethane (2 mL) was stirred for 30 min at room temperature in the presence of 4A molecular sieves (200 mg). The reaction mixture was acidified with aceti...
10.6084/m9.figshare.5104873.v1
null
Formaldehyde.Primary amine
Secondary amine
null
null
c1ccc2ncccc2c1.c1ccccc1
Other
ClC(C)Cl
null
16
C=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F>ClC(C)Cl>CNC(Cc1ccnc2ccccc12)(CC(C)(C)c1cc(F)ccc1OC)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-06a1b845d841460fa85679daee335f1f
CC(=O)OC(C)=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F>>COc1ccc(F)cc1C(C)(C)CC(Cc1ccnc2ccccc12)(NC(C)=O)C(F)(F)F
FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)N)(C)C)OC.C(C)(=O)OC(C)=O>>FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)NC(C)=O)(C)C)OC
CC(=O)O[C:27]([CH3:28])=[O:29].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3:12])[CH2:13][C:14]([CH2:15][c:16]1[cH:17][cH:18][n:19][c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]12)([NH2:26])[C:30]([F:31])([F:32])[F:33]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3...
CC(=O)OC(C)=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F
COc1ccc(F)cc1C(C)(C)CC(Cc1ccnc2ccccc12)(NC(C)=O)C(F)(F)F
null
null
ClC(C)Cl
Acylation
Aminolysis of esters
87d35e51b477fc9a658a6f307eb56d84c8879182772c9dd3a42ec0d584fd2684
627cbc0550c9f51ad0105d9fcf46677e8c93bed87ee95bfe69292a82550c95b7
c1ccc(CCCCc2ccnc3ccccc23)cc1
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[C:4]-[C:5](-[C:6])(-[NH2;D1;+0:7])-[C:8](-[F;D1;H0:9])(-[F;D1;H0:10])-[F;D1;H0:11]>>[C:4]-[C:5](-[C:6])(-[NH;D2;+0:7]-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3])-[C:8](-[F;D1;H0:9])(-[F;D1;H0:10])-[F;D1;H0:11]
74
[{"value": 74.0, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)NC(C)=O)(C)C)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73.5, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)NC(C)=O)(C)C)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
16
HOUR
A solution of 3-(5-fluoro-2-methoxy-phenyl)-3-methyl-1-quinolin-4-ylmethyl-1-trifluoromethyl-butylamine (42.0 mg, 0.1 mmol) in dichloroethane (4 mL) was treated with acetic anhydride (71 μL, 1.0 mmol). The mixture was stirred for 16 h at 85° C. and quenched with NaHCO3 (sat, 4 mL). Phases were separated and the aqueous...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccc2ncccc2c1
HO-
ClC(C)Cl
85
16
CC(=O)OC(C)=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F>ClC(C)Cl>COc1ccc(F)cc1C(C)(C)CC(Cc1ccnc2ccccc12)(NC(C)=O)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-27986a26fcae4b74a8276a0be92b4c2c
C=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F>>COc1ccc(F)cc1C(C)(C)CC(Cc1ccnc2ccccc12)(N(C)C)C(F)(F)F
C(#N)[BH3-].[Na+].FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)N)(C)C)OC.C=O.C(C)(=O)O>>FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)N(C)C)(C)C)OC
O=[CH2:27].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3:12])[CH2:13][C:14]([CH2:15][c:16]1[cH:17][cH:18][n:19][c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]12)([NH2:26])[C:29]([F:30])([F:31])[F:32]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][c:9]1[C:10]([CH3:11])([CH3:12])[CH2:13][C:14](...
C=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F
COc1ccc(F)cc1C(C)(C)CC(Cc1ccnc2ccccc12)(N(C)C)C(F)(F)F
null
null
C(C)#N
Heteroatom Alkylation and Arylation
Eschweiler-Clarke Primary Amine Methylation
5bc40be4d4b4346801fbfcec480fec37de3ff2eecebe2990b3686fa4792d12b6
5cdbf447f632627824e84e0bcac2293ea9ebd70c19b0d56dea90691653b444c7
c1ccc(CCCCc2ccnc3ccccc23)cc1
O=[CH2;D1;+0:1].[C:2]-[C:3](-[C:4])(-[NH2;D1;+0:5])-[C:6](-[F;D1;H0:7])(-[F;D1;H0:8])-[F;D1;H0:9]>>[C:2]-[C:3](-[C:4])(-[N;H0;D3;+0:5](-[C;D1;H3:10])-[CH3;D1;+0:1])-[C:6](-[F;D1;H0:7])(-[F;D1;H0:8])-[F;D1;H0:9]
28
[{"value": 28.0, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)N(C)C)(C)C)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 27.9, "product": "FC=1C=CC(=C(C1)C(CC(C(F)(F)F)(CC1=CC=NC2=CC=CC=C12)N(C)C)(C)C)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
HOUR
A solution of 3-(5-Fluoro-2-methoxy-phenyl)-3-methyl-1-quinolin-4-ylmethyl-1-trifluoromethyl-butylamine (42.0 mg, 0.1 mmol) and the formaldehyde (1.49 ml, 20 mmol) in acetonitrile (2 ml) was stirred for 30 minutes at room temperature. The reaction mixture was acidified with acetic acid (57 μL, 1.0 mmol) and treated wit...
10.6084/m9.figshare.5104873.v1
null
Formaldehyde.Primary amine
Tertiary amine
null
null
c1ccccc1.c1ccc2ncccc2c1
null
C(C)#N
null
15
C=O.COc1ccc(F)cc1C(C)(C)CC(N)(Cc1ccnc2ccccc12)C(F)(F)F>C(C)#N>COc1ccc(F)cc1C(C)(C)CC(Cc1ccnc2ccccc12)(N(C)C)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-701b5f1c918649d0a0cd6ae9ff8a1478
BrCc1ccccc1.CCN(CC)C(=O)c1ccc(C(Br)=C2CCN(C(=O)OC(C)(C)C)CC2)cc1>>CCN(CC)C(=O)c1ccc(C(Br)=C2CCN(Cc3ccccc3)CC2)cc1
C(C)(C)(C)OC(=O)N1CCC(CC1)=C(C1=CC=C(C=C1)C(N(CC)CC)=O)Br.C(=O)(C(F)(F)F)O.C(C1=CC=CC=C1)Br.C(C)N(CC)CC>>C(C)N(C(C1=CC=C(C=C1)C(=C1CCN(CC1)CC1=CC=CC=C1)Br)=O)CC
Br[CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23][cH:24]1.CC(C)(C)OC(=O)[N:17]1[CH2:16][CH2:15][C:14](=[C:12]([c:11]2[cH:10][cH:9][c:8]([C:6]([N:3]([CH2:2][CH3:1])[CH2:4][CH3:5])=[O:7])[cH:28][cH:27]2)[Br:13])[CH2:26][CH2:25]1>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([C:12]([Br:13])=[C:14]...
BrCc1ccccc1.CCN(CC)C(=O)c1ccc(C(Br)=C2CCN(C(=O)OC(C)(C)C)CC2)cc1
CCN(CC)C(=O)c1ccc(C(Br)=C2CCN(Cc3ccccc3)CC2)cc1
null
null
ClCCl
Heteroatom Alkylation and Arylation
OtherReaction
2748de0f66b24d9234b7038da32a953a331d785cf6b99b2cb684608e577382cc
a8bb195a563e3d75cf4b5698f17ee0104c6036dda9c0d819e472675fa1d5becb
C(=C1CCN(Cc2ccccc2)CC1)c1ccccc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:5]1-[C:6]-[C:7]-[C:8](=[C:9])-[C:10]-[C:11]-1>>[C:9]=[C:8]1-[C:7]-[C:6]-[N;H0;D3;+0:5](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:11]-[C:10]-1
64
[{"value": 64.0, "product": "C(C)N(C(C1=CC=C(C=C1)C(=C1CCN(CC1)CC1=CC=CC=C1)Br)=O)CC", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
Compound 6, prepared in Example 1 (v) above (6.122 g, 13.4 mmoL), was treated with TFA (13 mL) in dichloromethane (80 mL) at room temperature. After 2 h, the reaction mixture was washed with 2M sodium hydroxide (25 mL) and the organic layer was separated. The organic layer was dried (MgSO), filtered and concentrated. T...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carbamic ester.Ether.Boc
Tertiary amine
C1CC[NH]CC1
C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1.c1ccccc1
HBr
ClCCl
0
2
BrCc1ccccc1.CCN(CC)C(=O)c1ccc(C(Br)=C2CCN(C(=O)OC(C)(C)C)CC2)cc1>ClCCl>CCN(CC)C(=O)c1ccc(C(Br)=C2CCN(Cc3ccccc3)CC2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7993330f56544394abc27c1cca50f87f
COC(=O)c1cc(OC)cc(C(=O)OC)c1>>COC(=O)c1cc(OC)cc(C(=O)O)c1
COC(C1=CC(C(=O)OC)=CC(=C1)OC)=O.[OH-].[Na+]>>COC(C1=CC(C(=O)O)=CC(=C1)OC)=O
C[O:14][C:12]([c:11]1[cH:10][c:7]([O:8][CH3:9])[cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:15]1)=[O:13]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([O:8][CH3:9])[cH:10][c:11]([C:12](=[O:13])[OH:14])[cH:15]1
COC(=O)c1cc(OC)cc(C(=O)OC)c1
COC(=O)c1cc(OC)cc(C(=O)O)c1
null
null
CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccccc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4]>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4]
75.1
[{"value": 75.0, "product": "COC(C1=CC(C(=O)O)=CC(=C1)OC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.1, "product": "COC(C1=CC(C(=O)O)=CC(=C1)OC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A suspension of dimethyl-5-methoxy-isophthalate (6.4 g, 28.5 mmol) in methanol (143 mL) was treated with 1 N sodium hydroxide (25.6 mL, 25.6 mmol). The reaction was left stirring overnight at room temperature. After the solution was concentrated, the residue was dissolved in water and transferred to a separatory funnel...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1
Other
CO
null
8
COC(=O)c1cc(OC)cc(C(=O)OC)c1>CO>COC(=O)c1cc(OC)cc(C(=O)O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-49f67a00773e439ca0f77853451bc9f9
COC(=O)c1cc(OC)cc(C(N)=O)c1>>COC(=O)c1cc(C#N)cc(OC)c1
COC(C1=CC(C(=O)N)=CC(=C1)OC)=O.N1=CC=CC=C1.FC(C(=O)OC(C(F)(F)F)=O)(F)F>>COC(C1=CC(=CC(=C1)OC)C#N)=O
O=[C:8]([c:7]1[cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:14][c:11]([O:12][CH3:13])[cH:10]1)[NH2:9]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([C:8]#[N:9])[cH:10][c:11]([O:12][CH3:13])[cH:14]1
COC(=O)c1cc(OC)cc(C(N)=O)c1
COC(=O)c1cc(C#N)cc(OC)c1
null
null
ClCCl
Miscellaneous
OtherReaction
5094e9d814705bbdc421edbf7e9198e499e70e93916e2cec6eefbc82d1ba5440
32b9893bcb5223559a9d02852f8392cf6473aacfb044a52ba4e9cb9c29edb170
c1ccccc1
O=[C;H0;D3;+0:1](-[NH2;D1;+0:2])-[c:3](:[c:4]):[c:5]>>[N;H0;D1;+0:2]#[C;H0;D2;+0:1]-[c:3](:[c:4]):[c:5]
98.6
[{"value": 98.0, "product": "COC(C1=CC(=CC(=C1)OC)C#N)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.6, "product": "COC(C1=CC(=CC(=C1)OC)C#N)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
20
MINUTE
A suspension of 5-methoxy-isophthalamic acid methyl ester (4.0 g, 19.1 mmol) in a dichloromethane (80 mL) at 0° C. was treated with pyridine (6.3 mL, 77.0 mmol) and then trifluoroacetic anhydride drop-wise (6.5 mL, 46 mmol). The reaction was stirred at 0° C. for 20 min. and then stirred overnight at room temperature. T...
10.6084/m9.figshare.5104873.v1
null
Primary amide
Nitrile
null
null
c1ccccc1
HO-
ClCCl
0
0.333333
COC(=O)c1cc(OC)cc(C(N)=O)c1>ClCCl>COC(=O)c1cc(C#N)cc(OC)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a4151484a7b049b5ab77f711a10b50be
COC(=O)c1cc(C#N)cc(OC)c1>>COc1cc(C#N)cc(C(=O)O)c1
COC(C1=CC(=CC(=C1)OC)C#N)=O.[OH-].[Li+]>>C(#N)C=1C=C(C(=O)O)C=C(C1)OC
C[O:12][C:10]([c:9]1[cH:8][c:5]([C:6]#[N:7])[cH:4][c:3]([O:2][CH3:1])[cH:13]1)=[O:11]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([C:6]#[N:7])[cH:8][c:9]([C:10](=[O:11])[OH:12])[cH:13]1
COC(=O)c1cc(C#N)cc(OC)c1
COc1cc(C#N)cc(C(=O)O)c1
null
null
C1CCOC1
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccccc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4]>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4]
77
[{"value": 77.0, "product": "C(#N)C=1C=C(C(=O)O)C=C(C1)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.5, "product": "C(#N)C=1C=C(C(=O)O)C=C(C1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
75
CELSIUS
2
HOUR
A solution of 3-cyano-5-methoxy-benzoic acid methyl ester (3.4 g, 18.7 mmol) in THF (45 mL) was treated with 0.5 N lithium hydroxide (45 mL, 22.4 mmol). The reaction was stirred at 75° C. for 2 h and then the solvent was removed in vacuo. The residue was dissolved in a small amount of water and then acidified (pH 2) by...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1
Other
C1CCOC1
75
2
COC(=O)c1cc(C#N)cc(OC)c1>C1CCOC1>COc1cc(C#N)cc(C(=O)O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5b79f67932a94e14accfc8c088e94cde
Fc1cc(Br)cc(-n2ccnc2)c1>>N#Cc1cc(F)cc(-n2ccnc2)c1
FC=1C=C(C=C(C1)Br)N1C=NC=C1.CN(C)C=O.[Br-]>>FC=1C=C(C=C(C1)C#N)N1C=NC=C1
Br[c:3]1[cH:4][c:5]([F:6])[cH:7][c:8](-[n:9]2[cH:10][cH:11][n:12][cH:13]2)[cH:14]1>>[N:1]#[C:2][c:3]1[cH:4][c:5]([F:6])[cH:7][c:8](-[n:9]2[cH:10][cH:11][n:12][cH:13]2)[cH:14]1
Fc1cc(Br)cc(-n2ccnc2)c1
N#Cc1cc(F)cc(-n2ccnc2)c1
null
[C-]#N.[Zn+2].[C-]#N.C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1
null
Miscellaneous
OtherReaction
3ae4da8b7f110de99cf8afc091b6f0c8540050148e425770f8030bce1480042c
73a96fe5e833259ca394a42f82d6cc2ee7231bcde92d95030d2893b90c3fef76
c1ccc(-n2ccnc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]>>[N;D1;H0:6]#[C:7]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
80
CELSIUS
null
null
A solution of 3-fluoro-5-bromo-(1H-imidazol-1-yl)-benzene in DMF (36 mL) was treated with zinc cyanide and tetrakis(triphenylphosphine)palladium(0). The reaction mixture was heated under an argon atmosphere for 18 h at 80° C. when GC-MS indicated complete disappearance of starting bromide and presence of product molecu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Nitrile
c1ccccc1
c1ccccc1
c1ccccc1.c1c[nH]cn1
Br-
[C-]#N.[Zn+2].[C-]#N.C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1
80
null
Fc1cc(Br)cc(-n2ccnc2)c1>[C-]#N.[Zn+2].[C-]#N.C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1>N#Cc1cc(F)cc(-n2ccnc2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-31068ea7e3ba4a8ab43d092f97804004
CC(C)(C)OC(=O)N1CCCCC1C(=O)O.N>>CC(C)(C)OC(=O)N1CCCCC1C#N
N.C(C)N(CC)CC.C(C)(C)(C)OC(=O)N1C(CCCC1)C(=O)O.ClC(=O)OCC>>C(C)(C)(C)OC(=O)N1C(CCCC1)C#N
O=[C:14](O)[CH:13]1[N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][CH2:10][CH2:11][CH2:12]1.[NH3:15]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH:13]1[C:14]#[N:15]
CC(C)(C)OC(=O)N1CCCCC1C(=O)O.N
CC(C)(C)OC(=O)N1CCCCC1C#N
null
null
C1CCOC1
Miscellaneous
OtherReaction
6daec5e71bbc82d6d1305b776bb14d16edf8cd607701702401322171e2ae3591
fe1b71f0ae392b327c6a5cc3c2c245a8e15960efcad58e19a65ce9bcf5ea8243
C1CCNCC1
O-[C;H0;D3;+0:1](=O)-[C:2](-[C:3])-[#7:4](-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:11])-[C:12].[NH3;D0;+0:13]>>[C:3]-[C:2](-[C;H0;D2;+0:1]#[N;H0;D1;+0:13])-[#7:4](-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:11])-[C:12]
80.4
[{"value": 74.0, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 80.4, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-20
CELSIUS
null
null
Piperidine-1,2-dicarboxylic acid-1-tert-butyl ester (12.8 g, 55.6 mmol) and THF (170 mL) were added to a 500 mL round bottom flask equipped with stir bar. The solution was cooled to −20° C. and triethylamine (10.1 mL, 72.3 mmol) was added followed by ethyl chloroformate (5.32 mL, 55.6 mmol). The resulting white precipi...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Nitrile
null
null
C1CC[NH]CC1
HO-
C1CCOC1
-20
null
CC(C)(C)OC(=O)N1CCCCC1C(=O)O.N>C1CCOC1>CC(C)(C)OC(=O)N1CCCCC1C#N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3edc9b2b8f3444c9ae70e7c1766ffe10
CC(C)(C)OC(=O)N1CCCCC1C(N)=O>>CC(C)(C)OC(=O)N1CCCCC1C#N
C(C(=O)Cl)(=O)Cl.C(C)(C)(C)OC(=O)N1C(CCCC1)C(N)=O.N1=CC=CC=C1.CN(C)C=O>>C(C)(C)(C)OC(=O)N1C(CCCC1)C#N
O=[C:14]([CH:13]1[N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][CH2:10][CH2:11][CH2:12]1)[NH2:15]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH:13]1[C:14]#[N:15]
CC(C)(C)OC(=O)N1CCCCC1C(N)=O
CC(C)(C)OC(=O)N1CCCCC1C#N
null
null
C(C)#N
Miscellaneous
OtherReaction
5094e9d814705bbdc421edbf7e9198e499e70e93916e2cec6eefbc82d1ba5440
32b9893bcb5223559a9d02852f8392cf6473aacfb044a52ba4e9cb9c29edb170
C1CCNCC1
O=[C;H0;D3;+0:1](-[NH2;D1;+0:2])-[C:3](-[C:4])-[#7:5](-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12])-[C:13]>>[C:4]-[C:3](-[C;H0;D2;+0:1]#[N;H0;D1;+0:2])-[#7:5](-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12])-[C:13]
97.4
[{"value": 97.0, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.4, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-5
CELSIUS
null
null
Acetonitrile (220 mL) and DMF (3.82 mL, 49.4 mmol) were added to a 500 mL round bottom flask equipped with stir bar. Cooled the mixture down to −5° C. and to it added oxalyl chloride (24.7 mL, 49.4 mmol, 2 M dichloromethane). The resulting mixture was stirred for 15 min. This was followed by addition of solution of 2-c...
10.6084/m9.figshare.5104873.v1
null
Primary amide
Nitrile
null
null
C1CC[NH]CC1
HO-
C(C)#N
-5
null
CC(C)(C)OC(=O)N1CCCCC1C(N)=O>C(C)#N>CC(C)(C)OC(=O)N1CCCCC1C#N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a9abdd14d13e4aaab88e0d197f3e87dd
N#Cc1cccs1.NO>>N=C(NO)c1cccs1
C(C)O.S1C(=CC=C1)C#N.Cl.NO.[OH-].[Na+]>>ONC(=N)C=1SC=CC1
[N:1]#[C:2][c:5]1[cH:6][cH:7][cH:8][s:9]1.[NH2:3][OH:4]>>[NH:1]=[C:2]([NH:3][OH:4])[c:5]1[cH:6][cH:7][cH:8][s:9]1
N#Cc1cccs1.NO
N=C(NO)c1cccs1
null
null
ClCCl.O
Heteroatom Alkylation and Arylation
N-hydroxyimidamide from nitrile and hydroxylamine
08a01a2d1cd9346f7b3dddbfcbf8124b349e5763794287a4a1b9ee287b4d6aa7
38c3b778e04536ea6155ce05fc7c4746354a32b3703099defb07490833e3a961
c1ccsc1
[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[#16;a:5]:[c:6].[NH2;D1;+0:7]-[O;D1;H1:8]>>[NH;D1;+0:1]=[C;H0;D3;+0:2](-[NH;D2;+0:7]-[O;D1;H1:8])-[c:3](:[c:4]):[#16;a:5]:[c:6]
88
[{"value": 88.0, "product": "ONC(=N)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
To an ethanol (5 mL) solution of 2-thiophenecarbonitrile (525.5 mg, 5 mmol), 5 M hydroxylamine hydrochloride (1.1 mL) and 1 M sodium hydroxide (5.5 mL) were added. After the reaction mixture was heated at 80° C. for 3 h, water and dichloromethane were added. The organic layer was dried, concentrated and triturated with...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Primary amine
Secondary amine
null
null
c1ccsc1
null
ClCCl.O
80
null
N#Cc1cccs1.NO>ClCCl.O>N=C(NO)c1cccs1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-08c518ddca984a52aaff357143fecc4d
CCc1cccc(C#N)c1.NO>>CCc1cccc(C(=N)NO)c1
C(C)C=1C=C(C#N)C=CC1.Cl.NO.[OH-].[Na+]>>C(C)C=1C=C(C(=N)NO)C=CC1
[CH3:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8]#[N:9])[cH:12]1.[NH2:10][OH:11]>>[CH3:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8](=[NH:9])[NH:10][OH:11])[cH:12]1
CCc1cccc(C#N)c1.NO
CCc1cccc(C(=N)NO)c1
null
null
C(C)O
Heteroatom Alkylation and Arylation
N-hydroxyimidamide from nitrile and hydroxylamine
08a01a2d1cd9346f7b3dddbfcbf8124b349e5763794287a4a1b9ee287b4d6aa7
38c3b778e04536ea6155ce05fc7c4746354a32b3703099defb07490833e3a961
c1ccccc1
[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[c:5].[NH2;D1;+0:6]-[O;D1;H1:7]>>[NH;D1;+0:1]=[C;H0;D3;+0:2](-[NH;D2;+0:6]-[O;D1;H1:7])-[c:3](:[c:4]):[c:5]
46
[{"value": 46.0, "product": "C(C)C=1C=C(C(=N)NO)C=CC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
3-Ethyl-benzonitrile (400 mg, 3.05 mmol) with 5 M hydroxylamine hydrochloride (0.61 mL) and 1 M sodium hydroxide (3.05 mL) in ethanol (3 mL) were stirred at room temperature for 60 h. Work up as in example 4 afforded 230 mg (46%) of 3-ethyl-N-hydroxy-benzamidine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Nitrile.Primary amine
Secondary amine
null
null
c1ccccc1
null
C(C)O
null
null
CCc1cccc(C#N)c1.NO>C(C)O>CCc1cccc(C(=N)NO)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-36199a77d7744869bd14dc8e316823d6
CN(C)C=O.Cc1cc[c]([Mg][Br])nc1>>Cc1ccc(C=O)nc1
CC=1C=CC(=NC1)[Mg]Br.C1CCOC1.CN(C)C=O>>CC=1C=CC(=NC1)C=O
CN(C)[CH:6]=[O:7].[Br][Mg][c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:9][n:8]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([CH:6]=[O:7])[n:8][cH:9]1
CN(C)C=O.Cc1cc[c]([Mg][Br])nc1
Cc1ccc(C=O)nc1
null
null
null
C-C Coupling
OtherReaction
9604d2e886e0bc8c47ad2945f9a5a6e743d4e4a6997677963260fd89592474cd
a58e2418b13d3d8c24c7fc0b5536d7cd7f384640d0a25ca1c1aac16b0b551ae5
c1ccncc1
C-N(-C)-[CH;D2;+0:1]=[O;D1;H0:2].[Br]-[Mg]-[c;H0;D3;+0:3](:[#7;a:4]:[c:5]):[c:6]:[c:7]>>[O;D1;H0:2]=[CH;D2;+0:1]-[c;H0;D3;+0:3](:[#7;a:4]:[c:5]):[c:6]:[c:7]
62.6
[{"value": 62.6, "product": "CC=1C=CC(=NC1)C=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To the 0.25 M 5-methyl-2-pyridinylmagnesium bromide of THF solution (20 mL, 5 mmol), DMF (0.773 mL, 10 mmol) was added at room temperature under argon. The reaction mixture was stirred for 10 min. and concentrated in vacuo. The residue was quenched with saturated ammonium chloride and dichloromethane. The organic layer...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Tertiary amide
Aldehyde
c1ccncc1
c1ccncc1
c1ccncc1
HBr.Mg
null
null
0.166667
CN(C)C=O.Cc1cc[c]([Mg][Br])nc1>>Cc1ccc(C=O)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cdf2fac1990c44f1be6a980ba0fd2b04
CN(C)C=O.Cc1ccn[c]([Mg][Br])c1>>Cc1ccnc(C=O)c1
CC1=CC(=NC=C1)[Mg]Br.C1CCOC1.CN(C)C=O>>CC1=CC(=NC=C1)C=O
CN(C)[CH:7]=[O:8].[Br][Mg][c:6]1[n:5][cH:4][cH:3][c:2]([CH3:1])[cH:9]1>>[CH3:1][c:2]1[cH:3][cH:4][n:5][c:6]([CH:7]=[O:8])[cH:9]1
CN(C)C=O.Cc1ccn[c]([Mg][Br])c1
Cc1ccnc(C=O)c1
null
null
null
C-C Coupling
OtherReaction
9604d2e886e0bc8c47ad2945f9a5a6e743d4e4a6997677963260fd89592474cd
a58e2418b13d3d8c24c7fc0b5536d7cd7f384640d0a25ca1c1aac16b0b551ae5
c1ccncc1
C-N(-C)-[CH;D2;+0:1]=[O;D1;H0:2].[Br]-[Mg]-[c;H0;D3;+0:3](:[#7;a:4]:[c:5]):[c:6]:[c:7]>>[O;D1;H0:2]=[CH;D2;+0:1]-[c;H0;D3;+0:3](:[#7;a:4]:[c:5]):[c:6]:[c:7]
71.5
[{"value": 71.5, "product": "CC1=CC(=NC=C1)C=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Methyl-pyridine-2-carbaldehyde (433 mg, 71.5%) was obtained from 0.25 M 4-methyl-2-pyridinylmagnesium bromide of THF solution (20 mL, 5 mmol) with DMF (0.773 mL, 10 mmol) at room temperature under argon. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Tertiary amide
Aldehyde
c1ccncc1
c1ccncc1
c1ccncc1
HBr.Mg
null
null
null
CN(C)C=O.Cc1ccn[c]([Mg][Br])c1>>Cc1ccnc(C=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fafd068689ee495580217a21665ecd92
CN(C)C=O.Cc1cccn[c]1[Mg][Br]>>Cc1cccnc1C=O
CC=1C(=NC=CC1)[Mg]Br.C1CCOC1.CN(C)C=O>>CC=1C(=NC=CC1)C=O
CN(C)[CH:8]=[O:9].[Br][Mg][c:7]1[c:2]([CH3:1])[cH:3][cH:4][cH:5][n:6]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]=[O:9]
CN(C)C=O.Cc1cccn[c]1[Mg][Br]
Cc1cccnc1C=O
null
null
null
C-C Coupling
OtherReaction
9604d2e886e0bc8c47ad2945f9a5a6e743d4e4a6997677963260fd89592474cd
a58e2418b13d3d8c24c7fc0b5536d7cd7f384640d0a25ca1c1aac16b0b551ae5
c1ccncc1
C-N(-C)-[CH;D2;+0:1]=[O;D1;H0:2].[Br]-[Mg]-[c;H0;D3;+0:3](:[#7;a:4]:[c:5]):[c:6](-[C;D1;H3:7]):[c:8]>>[C;D1;H3:7]-[c:6](:[c:8]):[c;H0;D3;+0:3](-[CH;D2;+0:1]=[O;D1;H0:2]):[#7;a:4]:[c:5]
33
[{"value": 33.0, "product": "CC=1C(=NC=CC1)C=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
3-Methyl-pyridine-2-carbaldehyde (200 mg, 33.0%) was obtained from 0.25 M 3-methyl-2-pyridinylmagnesium bromide of THF solution (20 mL, 5 mmol) with DMF (0.773 mL, 10 mmol) at room temperature under argon. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Tertiary amide
Aldehyde
c1ccncc1
c1ccncc1
c1ccncc1
HBr.Mg
null
null
null
CN(C)C=O.Cc1cccn[c]1[Mg][Br]>>Cc1cccnc1C=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e1f40f47ba5b4ffdb0a8c6d6403695d0
CCO.O=C(O)c1ccc(F)cn1>>CCOC(=O)c1ccc(F)cn1
FC=1C=CC(=NC1)C(=O)O.C(C)O.Cl>>C(C)OC(=O)C1=NC=C(C=C1)F
[CH3:1][CH2:2][OH:3].O[C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([F:10])[cH:11][n:12]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([F:10])[cH:11][n:12]1
CCO.O=C(O)c1ccc(F)cn1
CCOC(=O)c1ccc(F)cn1
null
null
O1CCOCC1
Protection
Esterification of Carboxylic Acids
070670f68a20c1021da94fabee54def4688122fb721af5f52cd5a03630845d0e
0d8a72b7375d91aa7263e766e03a3cb7c4fa91e27abcd590409ff03b98eed690
c1ccncc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#7;a:5]:[c:6].[C;D1;H3:7]-[C:8]-[OH;D1;+0:9]>>[C;D1;H3:7]-[C:8]-[O;H0;D2;+0:9]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#7;a:5]:[c:6]
49.3
[{"value": 49.3, "product": "C(C)OC(=O)C1=NC=C(C=C1)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
5-Fluoro-pyridine-2-carboxylic acid (200 mg, 1.13 mmol) was mixed with ethanol (6 mL) and 4 M HCl in dioxane (0.5 mL) at 90° C. for 20 h. The mixture was concentrated and mixed with saturated sodium carbonate and dichloromethane. The dichloromethane layer was washed with brine, dried to give 94 mg (49.3%) of 5-fluoro-p...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary alcohol
Ester
null
null
c1ccncc1
HO-
O1CCOCC1
null
null
CCO.O=C(O)c1ccc(F)cn1>O1CCOCC1>CCOC(=O)c1ccc(F)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f4e88c7a4f2f4535a5b7fe669b0b17f4
CCOC(=O)c1ccc(F)cn1>>O=Cc1ccc(F)cn1
C(C)OC(=O)C1=NC=C(C=C1)F.C1(=CC=CC=C1)C>>FC=1C=CC(=NC1)C=O
CCO[C:2](=[O:1])[c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][n:9]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([F:7])[cH:8][n:9]1
CCOC(=O)c1ccc(F)cn1
O=Cc1ccc(F)cn1
null
null
ClCCl.CC(C)C[AlH]CC(C)C
Reduction
OtherReaction
ec1c6c64dd9be73981e5a6c952ab740869d298b20e87e097e88e1179cc5bc6dc
33ddc7b9457742ba0a376f08a972e4f33779267f6f1fe15e3be786427ae9f4ec
c1ccncc1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#7;a:5]:[c:6]>>[O;D1;H0:2]=[CH;D2;+0:1]-[c:3](:[c:4]):[#7;a:5]:[c:6]
56.1
[{"value": 54.7, "product": "FC=1C=CC(=NC1)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 56.1, "product": "FC=1C=CC(=NC1)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To 5-fluoro-pyridine-2-carboxylic acid ethyl ester (94 mg, 0.556 mmol) in dichloromethane (4.0 mL), 1 M DIBAL in toluene (1.23 mL, 1.23 mmol) was added at room temperature and the mixture was stirred for 30 min. The reaction mixture was quenched with 2 M sodium carbonate and extracted with dichloromethane. The dichloro...
10.6084/m9.figshare.5104873.v1
null
Ester
Aldehyde
null
null
c1ccncc1
HO-
ClCCl.CC(C)C[AlH]CC(C)C
null
0.5
CCOC(=O)c1ccc(F)cn1>ClCCl.CC(C)C[AlH]CC(C)C>O=Cc1ccc(F)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5c1c154152fe45b2afb28915615593be
O=C(O)c1ccc(Cl)cn1>>O=Cc1ccc(Cl)cn1
ClC=1C=CC(=NC1)C(=O)O.C(C)O.Cl>>ClC=1C=CC(=NC1)C=O
O[C:2](=[O:1])[c:3]1[cH:4][cH:5][c:6]([Cl:7])[cH:8][n:9]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[cH:8][n:9]1
O=C(O)c1ccc(Cl)cn1
O=Cc1ccc(Cl)cn1
null
null
O1CCOCC1
Reduction
OtherReaction
78999da0d33b2c10ff8c3d41626c41ea14d2697ff6d1d7e5baf78453ec38592a
f41d7c101137b93550fdf296ceb4547d1ce640e4cbceb5b7b006723d153456c9
c1ccncc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#7;a:5]:[c:6]>>[O;D1;H0:2]=[CH;D2;+0:1]-[c:3](:[c:4]):[#7;a:5]:[c:6]
52
[{"value": 52.0, "product": "ClC=1C=CC(=NC1)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 39.8, "product": "ClC=1C=CC(=NC1)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
5-Chloro-pyridine-2-carboxylic acid ethyl ester (146 mg, 76.3%) was obtained obtained as described in Example 11 from 5-chloro-pyridine-2-carboxylic acid (200 mg, 1.03 mmol) with ethanol (3 mL) and 4M HCl in dioxane (0.5 mL) at 90° C. for 20 h. 5-Chloro-pyridine-2-carbaldehyde (58 mg, 52%) was obtained as described in ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Aldehyde
null
null
c1ccncc1
Other
O1CCOCC1
null
null
O=C(O)c1ccc(Cl)cn1>O1CCOCC1>O=Cc1ccc(Cl)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c969145559604c7d8937ea3bf6a22d15
COC(=O)C1CCCCN1.O=Cc1ccccn1>>COC(=O)C1CCCCN1Cc1ccccn1
C(C)(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+].Cl.N1C(C(=O)OC)CCCC1.N1=C(C=CC=C1)C=O.C(C)N(CC)CC.C([O-])([O-])=O.[Na+].[Na+]>>COC(=O)C1N(CCCC1)CC1=NC=CC=C1
[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:6][CH2:7][CH2:8][CH2:9][NH:10]1.O=[CH:11][c:12]1[cH:13][cH:14][cH:15][cH:16][n:17]1>>[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:6][CH2:7][CH2:8][CH2:9][N:10]1[CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][n:17]1
COC(=O)C1CCCCN1.O=Cc1ccccn1
COC(=O)C1CCCCN1Cc1ccccn1
null
null
ClC(C)Cl
Heteroatom Alkylation and Arylation
reductive amination
d0e659bc8d1e29e09a61320b4c537e66ad57335a51368c8bd48de9bdffa59372
2d03f38884b1fbb0c0d6e6f2de31afb25102fec87f347c3a123e064c1bfef0ad
c1ccc(CN2CCCCC2)nc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[C:6]-[C:7](-[C:8](=[O;D1;H0:9])-[#8:10]-[C;D1;H3:11])-[NH;D2;+0:12]-[C:13]-[C:14]>>[C:6]-[C:7](-[C:8](=[O;D1;H0:9])-[#8:10]-[C;D1;H3:11])-[N;H0;D3;+0:12](-[CH2;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5])-[C:13]-[C:14]
93.6
[{"value": 93.6, "product": "COC(=O)C1N(CCCC1)CC1=NC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.0, "product": "COC(=O)C1N(CCCC1)CC1=NC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
Methyl pipecolinate hydrochloride (9.0 g, 50 mmol) was mixed with pyridine-2-carbaldehyde (5.4 g, 50 mmol) and triethylamine (5.05 g, 50 mmol) in dichloroethane (180 mL) at room temperature. Sodium triacetoxyborohydride (14.8 g, 70 mmol) was added in one portion. After the reaction mixture was stirred at room temperatu...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccncc1
Other
ClC(C)Cl
null
1.5
COC(=O)C1CCCCN1.O=Cc1ccccn1>ClC(C)Cl>COC(=O)C1CCCCN1Cc1ccccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cd10f91b73694d80bba3c4a92731a1f1
Cc1cccc(C(=O)O)n1>>CC1CCCC(C(=O)O)N1
CC1=CC=CC(=N1)C(=O)O>>CC1CCCC(N1)C(=O)O
[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]([C:7](=[O:8])[OH:9])[n:10]1>>[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][CH:6]([C:7](=[O:8])[OH:9])[NH:10]1
Cc1cccc(C(=O)O)n1
CC1CCCC(C(=O)O)N1
null
[Pt](=O)=O
O.C(C)O
Reduction
OtherReaction
8a6c78a63989dd47e282eb33ae5ce6bfcead5defaa210963e9125c31297ee886
2b7f370a519e29b4dede190aa36b37f30822496e32f2c8bfa9736e631bde52e2
C1CCNCC1
[C;D1;H3:1]-[c;H0;D3;+0:2]1:[cH;D2;+0:3]:[cH;D2;+0:4]:[cH;D2;+0:5]:[c;H0;D3;+0:6](-[C:7](=[O;D1;H0:8])-[O;D1;H1:9]):[n;H0;D2;+0:10]:1>>[C;D1;H3:1]-[CH;D3;+0:2]1-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[CH;D3;+0:6](-[C:7](=[O;D1;H0:8])-[O;D1;H1:9])-[NH;D2;+0:10]-1
98.3
[{"value": 98.3, "product": "CC1CCCC(N1)C(=O)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.4, "product": "CC1CCCC(N1)C(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
DAY
6-Methyl-pyridine-2-carboxylic acid (4.11 g, 30 mmol) was mixed with platinum(IV) oxide (35 mg, 0.154 mmol) in ethanol (50 mL) and water (25 mL) and stirred under hydrogen for 3 days. The reaction mixture was filtered through the celite and concentrated to dry. The residue was triturated with diethyl ether to give 4.1 ...
10.6084/m9.figshare.5104873.v1
null
null
Secondary amine
c1ccncc1
C1CCNCC1
C1CCNCC1
null
[Pt](=O)=O.O.C(C)O
null
72
Cc1cccc(C(=O)O)n1>[Pt](=O)=O.O.C(C)O>CC1CCCC(C(=O)O)N1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ed65202826954bf3adb9a2a7abfbaabc
COC(=O)C1CC(O)CCN1C(=O)OC(C)(C)C>>COC(=O)C1CC(=O)CCN1C(=O)OC(C)(C)C
OS(=O)(=O)[O-].[Na+].COC(=O)C1N(CCC(C1)O)C(=O)OC(C)(C)C.CS(=O)C.C(C(=O)Cl)(=O)Cl>>COC(=O)C1N(CCC(C1)=O)C(=O)OC(C)(C)C
[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:6][CH:7]([OH:8])[CH2:9][CH2:10][N:11]1[C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:6][C:7](=[O:8])[CH2:9][CH2:10][N:11]1[C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18]
COC(=O)C1CC(O)CCN1C(=O)OC(C)(C)C
COC(=O)C1CC(=O)CCN1C(=O)OC(C)(C)C
null
null
ClCCl.CCN(CC)CC.C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
eb1454704a72f81f212192eafcb78e0711de77dd6074b9d7e49d38205debb755
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
O=C1CCNCC1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]1-[#7:5]-[C:6]-[C:7]-[CH;D3;+0:8](-[OH;D1;+0:9])-[C:10]-1>>[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]1-[#7:5]-[C:6]-[C:7]-[C;H0;D3;+0:8](=[O;H0;D1;+0:9])-[C:10]-1
88.2
[{"value": 88.0, "product": "COC(=O)C1N(CCC(C1)=O)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 88.2, "product": "COC(=O)C1N(CCC(C1)=O)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
1
HOUR
To a mixture of oxalyl chloride ((15 mL, 30 mmol, 2 M dichloromethane) in CH2Cl2 (100 mL) cooled to −78° C. was added DMSO (4.5 mL, 63.4 mmol). The mixture was stirred at this temperature for 1 h, after which 4-hydroxy-piperidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (2.0 g, 7.71 mmol dissolved in CH2...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1
null
ClCCl.CCN(CC)CC.C(Cl)Cl
-78
1
COC(=O)C1CC(O)CCN1C(=O)OC(C)(C)C>ClCCl.CCN(CC)CC.C(Cl)Cl>COC(=O)C1CC(=O)CCN1C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f98dd5e94fc24360a3b4c09c127afdb6
CC(C)(C)OC(=O)N1CCCCC1C(=O)O.N#Cc1cccc(C(=N)NO)c1>>CC(C)(C)OC(=O)N1CCCCC1c1nc(-c2cccc(C#N)c2)no1
C(C)(C)(C)OC(=O)N1C(CCCC1)C(=O)O.C(C)N(CC)CC.ClC(=O)OCC(C)C.C(#N)C=1C=C(C(=N)NO)C=CC1>>C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NC(=NO1)C1=CC(=CC=C1)C#N
O=[C:14](O)[CH:13]1[N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][CH2:10][CH2:11][CH2:12]1.[NH:15]=[C:16]([c:17]1[cH:18][cH:19][cH:20][c:21]([C:22]#[N:23])[cH:24]1)[NH:25][OH:26]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH:13]1[c:14]1[n:15][c:16](-[c:17]2[cH...
CC(C)(C)OC(=O)N1CCCCC1C(=O)O.N#Cc1cccc(C(=N)NO)c1
CC(C)(C)OC(=O)N1CCCCC1c1nc(-c2cccc(C#N)c2)no1
null
null
ClCCl.O.CN(C)C=O.C1CCOC1
Aromatic Heterocycle Formation
OtherReaction
2705d90bec25fbfd90e98961543fc48076d6c6e89a60f6012587bc2b1ce04b13
7a7b5724a99f7b1ff61b1937894d90e5ffd70f2e3f6ae2fa59809f82d476dd48
c1ccc(-c2noc(C3CCCCN3)n2)cc1
O-[C;H0;D3;+0:1](=O)-[C:2](-[C:3])-[#7:4](-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:11])-[C:12].[NH;D1;+0:13]=[C;H0;D3;+0:14](-[NH;D2;+0:15]-[OH;D1;+0:16])-[c;H0;D3;+0:17](:[c:18]:[c:19]):[c:20]:[c:21]>>[C:3]-[C:2](-[c;H0;D3;+0:1]1:[n;H0;D2;+0:13]:[c;H0;D3;+0:14](-[c;H0;D3;+0:17](:[c:18]:[...
98.5
[{"value": 98.4, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NC(=NO1)C1=CC(=CC=C1)C#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.5, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NC(=NO1)C1=CC(=CC=C1)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
45
MINUTE
To a mixture of piperidine-1,2-dicarboxylic acid 1-tert-butyl ester (5.32 g, 23.2 mmol) and triethylamine (4.04 g, 40 mmol) in THF (50 mL), isobutyl chloroformate (3.0 mL, 25.5 mmol) was added dropwise. After the mixture was stirred at room temperature for 45 min, 3-cyano-N-hydroxy-benzamidine (3.7 g, 23.2 mmol) and DM...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
null
null
c1ncon1
C1CC[NH]CC1.c1ncon1.c1ccccc1
HO-
ClCCl.O.CN(C)C=O.C1CCOC1
null
0.75
CC(C)(C)OC(=O)N1CCCCC1C(=O)O.N#Cc1cccc(C(=N)NO)c1>ClCCl.O.CN(C)C=O.C1CCOC1>CC(C)(C)OC(=O)N1CCCCC1c1nc(-c2cccc(C#N)c2)no1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1699df2f672043e7829a1f11eb94148c
CC1CCCC(C(=O)O)N1C(=O)OC(C)(C)C.N#Cc1cccc(C(=N)NO)c1>>CC1CCCC(c2nc(-c3cccc(C#N)c3)no2)N1C(=O)OC(C)(C)C
C(C)(C)(C)OC(=O)N1C(CCCC1C)C(=O)O.ClC(=O)OCC(C)C.C(#N)C=1C=C(C(=N)NO)C=CC1.C(C)N(CC)CC>>C(C)(C)(C)OC(=O)N1C(CCCC1C)C1=NC(=NO1)C1=CC(=CC=C1)C#N
O=[C:7](O)[CH:6]1[CH2:5][CH2:4][CH2:3][CH:2]([CH3:1])[N:20]1[C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27].[NH:8]=[C:9]([c:10]1[cH:11][cH:12][cH:13][c:14]([C:15]#[N:16])[cH:17]1)[NH:18][OH:19]>>[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][CH:6]([c:7]2[n:8][c:9](-[c:10]3[cH:11][cH:12][cH:13][c:14]([C:15]#[N:16])[cH:17]3...
CC1CCCC(C(=O)O)N1C(=O)OC(C)(C)C.N#Cc1cccc(C(=N)NO)c1
CC1CCCC(c2nc(-c3cccc(C#N)c3)no2)N1C(=O)OC(C)(C)C
null
null
CN(C)C=O.C1CCOC1
Aromatic Heterocycle Formation
OtherReaction
2705d90bec25fbfd90e98961543fc48076d6c6e89a60f6012587bc2b1ce04b13
7a7b5724a99f7b1ff61b1937894d90e5ffd70f2e3f6ae2fa59809f82d476dd48
c1ccc(-c2noc(C3CCCCN3)n2)cc1
O-[C;H0;D3;+0:1](=O)-[C:2](-[C:3])-[#7:4](-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:11])-[C:12].[NH;D1;+0:13]=[C;H0;D3;+0:14](-[NH;D2;+0:15]-[OH;D1;+0:16])-[c;H0;D3;+0:17](:[c:18]:[c:19]):[c:20]:[c:21]>>[C:12]-[#7:4](-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:1...
48.6
[{"value": 46.2, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1C)C1=NC(=NO1)C1=CC(=CC=C1)C#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 48.6, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1C)C1=NC(=NO1)C1=CC(=CC=C1)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-[3-(3-Cyano-phenyl)-[1,2,4]oxadiazol-5-yl]-6-methyl-piperidine-1-carboxylic acid tert-butyl ester (340 mg, 46.2%) was prepared according to the procedure in Example 25 from 6-methyl-piperidine-1,2-dicarboxylic acid 1-tert-butyl ester (486 mg, 2 mmol) with isobutyl chloroformate (273.16 mg, 2.0 mmol) and triethylamine...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
null
null
c1ncon1
C1CC[NH]CC1.c1ncon1.c1ccccc1
HO-
CN(C)C=O.C1CCOC1
null
null
CC1CCCC(C(=O)O)N1C(=O)OC(C)(C)C.N#Cc1cccc(C(=N)NO)c1>CN(C)C=O.C1CCOC1>CC1CCCC(c2nc(-c3cccc(C#N)c3)no2)N1C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-58507d49889e46be85380f27529308d1
CC(C)(C)OC(=O)N1CCCCC1C(=N)NO.N#Cc1cccc(C(=O)Cl)c1>>CC(C)(C)OC(=O)N1CCCCC1c1noc(-c2cccc(C#N)c2)n1
CN(C)C=O.C(#N)C=1C=C(C(=O)Cl)C=CC1.C(C)(C)(C)OC(=O)N1C(CCCC1)C(NO)=N.C(C)N(CC)CC>>C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NOC(=N1)C1=CC(=CC=C1)C#N
O[NH:15][C:14]([CH:13]1[N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][CH2:10][CH2:11][CH2:12]1)=[NH:26].Cl[C:17](=[O:16])[c:18]1[cH:19][cH:20][cH:21][c:22]([C:23]#[N:24])[cH:25]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH:13]1[c:14]1[n:15][o:16][c:17](-[c:1...
CC(C)(C)OC(=O)N1CCCCC1C(=N)NO.N#Cc1cccc(C(=O)Cl)c1
CC(C)(C)OC(=O)N1CCCCC1c1noc(-c2cccc(C#N)c2)n1
null
null
ClCCl.C(C)(=O)OCC
Aromatic Heterocycle Formation
OtherReaction
35a949425cd7c777a41d64382aaf5f09103d9c9391a5f137dd482762a199998b
7f85aea1a67b85d56267cd6d88af12850e1092108f42124a342198b2ffd2e0d0
c1ccc(-c2nc(C3CCCCN3)no2)cc1
Cl-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c;H0;D3;+0:3](:[c:4]:[c:5]):[c:6]:[c:7].O-[NH;D2;+0:8]-[C;H0;D3;+0:9](=[NH;D1;+0:10])-[C:11](-[C:12])-[#7:13](-[C:14](=[O;D1;H0:15])-[#8:16]-[C:17](-[C;D1;H3:18])(-[C;D1;H3:19])-[C;D1;H3:20])-[C:21]>>[C:12]-[C:11](-[c;H0;D3;+0:9]1:[n;H0;D2;+0:8]:[o;H0;D2;+0:2]:[c;H0;D3;+0:1](-[c;H0;D...
22.3
[{"value": 22.3, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NOC(=N1)C1=CC(=CC=C1)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
In a 50 mL round bottom flask equipped with stir bar, added 2-(N-hydroxycarbamimidoyl)-piperidine-1-carboxylic acid tert-butyl ester (327 mg, 1.34 mmol), dichloromethane (5 mL) and triethylamine (0.56 mL, 4.03 mmol). To this stirred mixture was added a solution of 3-cyanobenzoyl chloride (222 mg, 1.34 mmol) in dichloro...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary amine
null
null
c1ncon1
C1CC[NH]CC1.c1ncon1.c1ccccc1
HCl
ClCCl.C(C)(=O)OCC
null
null
CC(C)(C)OC(=O)N1CCCCC1C(=N)NO.N#Cc1cccc(C(=O)Cl)c1>ClCCl.C(C)(=O)OCC>CC(C)(C)OC(=O)N1CCCCC1c1noc(-c2cccc(C#N)c2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c116e83071ab4eae99b80de63e45af7c
CC(C)(C)OC(=O)N1CCCCC1C(=N)NO.COc1ccc(C#N)c(C(=O)O)c1>>COc1cc(C#N)cc(-c2nc(C3CCCCN3C(=O)OC(C)(C)C)no2)c1
C(#N)C1=C(C(=O)O)C=C(C=C1)OC.CCN=C=NCCCN(C)C.C=1C=CC2=C(C1)N=NN2O.C(C)(C)(C)OC(=O)N1C(CCCC1)C(NO)=N>>C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NOC(=N1)C1=CC(=CC(=C1)OC)C#N
[NH:11]=[C:12]([CH:13]1[CH2:14][CH2:15][CH2:16][CH2:17][N:18]1[C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])[NH:26][OH:27].O=[C:10](O)[c:9]1[c:5]([C:6]#[N:7])[cH:8][cH:4][c:3]([O:2][CH3:1])[cH:28]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([C:6]#[N:7])[cH:8][c:9](-[c:10]2[n:11][c:12]([CH:13]3[CH2:14][CH2:15][CH2:16][CH2...
CC(C)(C)OC(=O)N1CCCCC1C(=N)NO.COc1ccc(C#N)c(C(=O)O)c1
COc1cc(C#N)cc(-c2nc(C3CCCCN3C(=O)OC(C)(C)C)no2)c1
null
null
CN(C)C=O.C(C)(=O)OCC
Aromatic Heterocycle Formation
OtherReaction
fb0af6d623a6fb0dc430126834eabf3f72dc4d55326f21657754c4c7ce40679a
7a7b5724a99f7b1ff61b1937894d90e5ffd70f2e3f6ae2fa59809f82d476dd48
c1ccc(-c2nc(C3CCCCN3)no2)cc1
O-[C;H0;D3;+0:1](=O)-[c;H0;D3;+0:2]1:[c:3]:[c:4](-[#8:5]):[cH;D2;+0:6]:[cH;D2;+0:7]:[c;H0;D3;+0:8]:1-[C:9]#[N;D1;H0:10].[C:11]-[C:12](-[C;H0;D3;+0:13](=[NH;D1;+0:14])-[NH;D2;+0:15]-[OH;D1;+0:16])-[#7:17](-[C:18](=[O;D1;H0:19])-[#8:20]-[C:21](-[C;D1;H3:22])(-[C;D1;H3:23])-[C;D1;H3:24])-[C:25]>>[#8:5]-[c:4]1:[c:3]:[c;H0;...
56
[{"value": 56.0, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NOC(=N1)C1=CC(=CC(=C1)OC)C#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 51.7, "product": "C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NOC(=N1)C1=CC(=CC(=C1)OC)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
135
CELSIUS
8
HOUR
DMF (2.0 mL) was added to a mixture of cyano-5-methoxybenzoic acid (160 mg, 0.90 mmol), EDCI (176 mg, 0.92 mmol), HOBt (124.3 mg, 0.92 mmol) and 2-(N-hydroxycarbamimidoyl)-piperidine-1-carboxylic acid tert-butyl ester (224 mg, 0.92 mmol) at room temperature and stirred overnight. The reaction mixture was diluted with e...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
null
c1ccccc1
c1ccccc1.c1ncon1
c1ccccc1.c1ncon1.C1CC[NH]CC1
HO-
CN(C)C=O.C(C)(=O)OCC
135
8
CC(C)(C)OC(=O)N1CCCCC1C(=N)NO.COc1ccc(C#N)c(C(=O)O)c1>CN(C)C=O.C(C)(=O)OCC>COc1cc(C#N)cc(-c2nc(C3CCCCN3C(=O)OC(C)(C)C)no2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-66a50e87870749f6a6723fc9a87525a5
CC(C)(C)OC(=O)N1CCCCC1c1nc(-c2cccc(C#N)c2)no1>>N#Cc1cccc(-c2noc(C3CCCCN3)n2)c1
C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NC(=NO1)C1=CC(=CC=C1)C#N>>N1C(CCCC1)C1=NC(=NO1)C=1C=C(C#N)C=CC1
CC(C)(C)OC(=O)[N:17]1[CH:12]([c:11]2[o:10][n:9][c:8](-[c:7]3[cH:6][cH:5][cH:4][c:3]([C:2]#[N:1])[cH:19]3)[n:18]2)[CH2:13][CH2:14][CH2:15][CH2:16]1>>[N:1]#[C:2][c:3]1[cH:4][cH:5][cH:6][c:7](-[c:8]2[n:9][o:10][c:11]([CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:17]3)[n:18]2)[cH:19]1
CC(C)(C)OC(=O)N1CCCCC1c1nc(-c2cccc(C#N)c2)no1
N#Cc1cccc(-c2noc(C3CCCCN3)n2)c1
null
null
C(=O)O
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc(-c2noc(C3CCCCN3)n2)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4](-[c:5](:[#7;a:6]):[#8;a:7]:[#7;a:8])-[C:9]>>[#7;a:6]:[c:5](-[C:4](-[C:9])-[NH;D2;+0:1]-[C:2]-[C:3]):[#8;a:7]:[#7;a:8]
77.4
[{"value": 73.4, "product": "N1C(CCCC1)C1=NC(=NO1)C=1C=C(C#N)C=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.4, "product": "N1C(CCCC1)C1=NC(=NO1)C=1C=C(C#N)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
45
CELSIUS
null
null
2-[3-(3-Cyano-phenyl)-[1,2,4]oxadiazol-5-yl]-piperidine-1-carboxylic acid tert-butyl ester (8.1 g) was mixed with 96% formic acid (80 mL) and heated at 45° C. for 1 h. The reaction mixture was concentrated in vacuo. The residue was quenched with saturated sodium bicarbonate and extracted with dichloromethane. The organ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccccc1.c1ncon1.C1CCNCC1
HO-
C(=O)O
45
null
CC(C)(C)OC(=O)N1CCCCC1c1nc(-c2cccc(C#N)c2)no1>C(=O)O>N#Cc1cccc(-c2noc(C3CCCCN3)n2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dbd37b52b58d4dac829cc80eb1f6e6a3
COc1cc(C#N)cc(-c2nc(C3CCCCN3C(=O)OC(C)(C)C)no2)c1>>COc1cc(C#N)cc(-c2nc(C3CCCCN3Cc3ccccn3)no2)c1
C(C)(C)(C)OC(=O)N1C(CCCC1)C1=NOC(=N1)C1=CC(=CC(=C1)OC)C#N.FC(C(=O)O)(F)F>>COC=1C=C(C#N)C=C(C1)C1=NC(=NO1)C1N(CCCC1)CC1=NC=CC=C1
O=[C:19](O[C:23]([CH3:21])([CH3:22])[CH3:24])[N:18]1[CH:13]([c:12]2[n:11][c:10](-[c:9]3[cH:8][c:5]([C:6]#[N:7])[cH:4][c:3]([O:2][CH3:1])[cH:28]3)[o:27][n:26]2)[CH2:14][CH2:15][CH2:16][CH2:17]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([C:6]#[N:7])[cH:8][c:9](-[c:10]2[n:11][c:12]([CH:13]3[CH2:14][CH2:15][CH2:16][CH2:17][N:18]3[CH2...
COc1cc(C#N)cc(-c2nc(C3CCCCN3C(=O)OC(C)(C)C)no2)c1
COc1cc(C#N)cc(-c2nc(C3CCCCN3Cc3ccccn3)no2)c1
null
null
ClCCl
Aromatic Heterocycle Formation
OtherReaction
de7153b84dda2e90c71480994df0a3f3b8dc2f891c32890ceec26a6aefcdf10b
2c72fed15cc3edd74b0482c8ecd787e13465f4faff387e244477a633fd9b8e38
c1ccc(-c2nc(C3CCCCN3Cc3ccccn3)no2)cc1
O=[C;H0;D3;+0:1](-O-[C;H0;D4;+0:2](-[CH3;D1;+0:3])(-[CH3;D1;+0:4])-[CH3;D1;+0:5])-[#7:6](-[C:7])-[C:8]>>[C:7]-[#7:6](-[CH2;D2;+0:1]-[c:9]1:[#7;a:10]:[cH;D2;+0:5]:[cH;D2;+0:2]:[cH;D2;+0:4]:[cH;D2;+0:3]:1)-[C:8]
null
[]
null
null
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null
To a solution of 2-[5-(3-cyano-5-methoxy-phenyl)-[1,2,4]oxadiazol-3-yl]-piperidine-1-carboxylic acid tert-butyl ester (162 mg, 0.42 mmol) in dichloromethane (4 mL) cooling in an ice-bath was added trifluoroacetic acid (2 mL). The ice-bath was removed after 30 min. and then left stirring for an additional hour. After th...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
null
null
c1ccncc1
c1ccccc1.c1ncon1.C1CC[NH]CC1.c1ccncc1
null
ClCCl
null
null
COc1cc(C#N)cc(-c2nc(C3CCCCN3C(=O)OC(C)(C)C)no2)c1>ClCCl>COc1cc(C#N)cc(-c2nc(C3CCCCN3Cc3ccccn3)no2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6ab5f886a86e44dfae5f95c005cece48
ClCc1ccc2ccccc2n1.N#Cc1cccc(-c2noc(C3CCCCN3)n2)c1>>N#Cc1cccc(-c2noc(C3CCCCN3Cc3ccc4ccccc4n3)n2)c1
N1C(CCCC1)C1=NC(=NO1)C=1C=C(C#N)C=CC1.Cl.ClCC1=NC2=CC=CC=C2C=C1.C(C)(C)N(CC)C(C)C.Cl>>N1=C(C=CC2=CC=CC=C12)CN1C(CCCC1)C1=NC(=NO1)C=1C=C(C#N)C=CC1
Cl[CH2:18][c:19]1[cH:20][cH:21][c:22]2[cH:23][cH:24][cH:25][cH:26][c:27]2[n:28]1.[N:1]#[C:2][c:3]1[cH:4][cH:5][cH:6][c:7](-[c:8]2[n:9][o:10][c:11]([CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:17]3)[n:29]2)[cH:30]1>>[N:1]#[C:2][c:3]1[cH:4][cH:5][cH:6][c:7](-[c:8]2[n:9][o:10][c:11]([CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16]...
ClCc1ccc2ccccc2n1.N#Cc1cccc(-c2noc(C3CCCCN3)n2)c1
N#Cc1cccc(-c2noc(C3CCCCN3Cc3ccc4ccccc4n3)n2)c1
null
null
O.CCOCC.CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(-c2noc(C3CCCCN3Cc3ccc4ccccc4n3)n2)cc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[#7;a:6]:[c:7](-[C:8](-[C:9])-[NH;D2;+0:10]-[C:11]-[C:12]):[#8;a:13]:[#7;a:14]>>[#7;a:6]:[c:7](-[C:8](-[C:9])-[N;H0;D3;+0:10](-[CH2;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5])-[C:11]-[C:12]):[#8;a:13]:[#7;a:14]
null
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null
null
null
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3-(5-Piperidin-2-yl-[1,2,4]oxadiazol-3-yl)-benzonitrile (50.8 mg, 0.2 mmol) was mixed with 2-(chloromethyl)quinoline monohydrochloride (47.1 mg, 0.22 mmol) and diisopropylethylamine (129.3 mg, 1.0 mmol) in DMF (2 mL) at 80° C. for 20 h. The reaction mixture was poured into water and extracted with dichloromethane. The ...
10.6084/m9.figshare.5104873.v1
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Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccccc1.c1ncon1.C1CC[NH]CC1.c1ccc2ncccc2c1
HCl
O.CCOCC.CN(C)C=O
null
null
ClCc1ccc2ccccc2n1.N#Cc1cccc(-c2noc(C3CCCCN3)n2)c1>O.CCOCC.CN(C)C=O>N#Cc1cccc(-c2noc(C3CCCCN3Cc3ccc4ccccc4n3)n2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5aa70eb55f574960b7a7ce073d20565d
COC(=O)C1CCCCN1Cc1ccccn1.COc1cccc(C(=N)NO)c1>>COc1cccc(-c2noc(C3CCCCN3Cc3ccccn3)n2)c1
COC(=O)C1N(CCCC1)CC1=NC=CC=C1.ONC(C1=CC(=CC=C1)OC)=N.CC(C)([O-])C.[Na+]>>COC=1C=C(C=CC1)C1=NOC(=N1)C1N(CCCC1)CC1=NC=CC=C1
CO[C:11](=O)[CH:12]1[CH2:13][CH2:14][CH2:15][CH2:16][N:17]1[CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23][n:24]1.[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8]([NH:9][OH:10])=[NH:25])[cH:26]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7](-[c:8]2[n:9][o:10][c:11]([CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16][N:17]3[CH2:18][c:19]3...
COC(=O)C1CCCCN1Cc1ccccn1.COc1cccc(C(=N)NO)c1
COc1cccc(-c2noc(C3CCCCN3Cc3ccccn3)n2)c1
null
null
ClCCl.C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
88b71cc25219a15819c3a3f01bd6e17c339fa66cdf2edd95092bad2351ca17df
b2e640ad6adb277738cae8a944067d998d1107d1f884bf69b59d55eb50b99f16
c1ccc(-c2noc(C3CCCCN3Cc3ccccn3)n2)cc1
C-O-[C;H0;D3;+0:1](=O)-[C:2](-[C:3])-[#7:4](-[C:5])-[C:6].[NH;D1;+0:7]=[C;H0;D3;+0:8](-[NH;D2;+0:9]-[OH;D1;+0:10])-[c;H0;D3;+0:11](:[c:12]:[c:13]):[c:14]:[c:15]>>[C:3]-[C:2](-[c;H0;D3;+0:1]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:8](-[c;H0;D3;+0:11](:[c:12]:[c:13]):[c:14]:[c:15]):[n;H0;D2;+0:9]:[o;H0;D2;+0:10]:1)-[#7:4](-[C:5])-[C...
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null
1-Pyridin-2-ylmethyl-piperidine-2-carboxylic acid methyl ester (50 mg, 0.213 mmol) was mixed with N-hydroxy-3-methoxy-benzamidine (29 mg, 0.174 mmol) and sodium tert-butoxide (19 mg, 0.20 mmol) in toluene (0.5 mL) in a sealed vial at 130° C. for 10 min. The reaction mixture was cooled down and diluted with dichlorometh...
10.6084/m9.figshare.5104873.v1
null
Ester.Secondary amine
null
null
c1ncon1
c1ccccc1.c1ncon1.C1CC[NH]CC1.c1ccncc1
HO-
ClCCl.C1(=CC=CC=C1)C
null
null
COC(=O)C1CCCCN1Cc1ccccn1.COc1cccc(C(=N)NO)c1>ClCCl.C1(=CC=CC=C1)C>COc1cccc(-c2noc(C3CCCCN3Cc3ccccn3)n2)c1