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-d90d6fe554fe4673b93da7fd41450434
CC(=O)CCl.COc1cccc(CC(=O)O)c1>>COc1cccc(C2=C(C)COC2=O)c1
COC=1C=C(C=CC1)CC(=O)O.ClCC(C)=O.C([O-])([O-])=O.[K+].[K+]>>COC=1C=C(C=CC1)C=1C(OCC1C)=O
O=[C:9]([CH3:10])[CH2:11]Cl.[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([CH2:8][C:13]([OH:12])=[O:14])[cH:15]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8]2=[C:9]([CH3:10])[CH2:11][O:12][C:13]2=[O:14])[cH:15]1
CC(=O)CCl.COc1cccc(CC(=O)O)c1
COc1cccc(C2=C(C)COC2=O)c1
null
null
C(C)#N.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
f037be6f9f026cd579480779429d9cffa8fcccf26ea746a7829725f430e584b0
937de3c41eef8eee72ef9ea5c72ba31c48840f648e4818110e3ac17f0dc2e4ad
O=C1OCC=C1c1ccccc1
Cl-[CH2;D2;+0:1]-[C;H0;D3;+0:2](=O)-[C;D1;H3:3].[O;D1;H0:4]=[C:5](-[OH;D1;+0:6])-[CH2;D2;+0:7]-[c:8](:[c:9]):[c:10]>>[C;D1;H3:3]-[C;H0;D3;+0:2]1=[C;H0;D3;+0:7](-[c:8](:[c:9]):[c:10])-[C:5](=[O;D1;H0:4])-[O;H0;D2;+0:6]-[CH2;D2;+0:1]-1
78.3
[{"value": 78.0, "product": "COC=1C=C(C=CC1)C=1C(OCC1C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.3, "product": "COC=1C=C(C=CC1)C=1C(OCC1C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 3-methoxyphenylacetic acid (3.32 g, 20 mmol), chloroacetone (2.02 g, 22 mmol) and potassium carbonate (6.07 g, 44 mmol) in acetonitrile (30 mL) was heated at reflux for 5 hours. The resultant mixture was cooled to room temperature, diluted with ethyl acetate (60 ml), filtered through a silica gel pad, and ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carboxylic acid.Ketone
Ester
null
C1=CCOC1
c1ccccc1.C1=CCOC1
HCl
C(C)#N.C(C)(=O)OCC
null
null
CC(=O)CCl.COc1cccc(CC(=O)O)c1>C(C)#N.C(C)(=O)OCC>COc1cccc(C2=C(C)COC2=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6d7f6c1d0fb4448c91e459ba3e7b5f52
COc1cccc(C2=C(C)C(O)=C(c3ccccc3F)C2=O)c1.NN>>COc1cccc(-c2c(C)c(Cc3ccccc3F)n[nH]c2=O)c1
FC1=C(C=CC=C1)C=1C(C(=C(C1O)C)C1=CC(=CC=C1)OC)=O.NN>>COC=1C=C(C=CC1)C=1C(NN=C(C1C)CC1=C(C=CC=C1)F)=O
O[C:11]1=[C:12]([c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]2[F:19])[C:22](=[O:23])[C:8]([c:7]2[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[cH:24]2)=[C:9]1[CH3:10].[NH2:20][NH2:21]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7](-[c:8]2[c:9]([CH3:10])[c:11]([CH2:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[F:19])[n:20][nH:21][c:22]2...
COc1cccc(C2=C(C)C(O)=C(c3ccccc3F)C2=O)c1.NN
COc1cccc(-c2c(C)c(Cc3ccccc3F)n[nH]c2=O)c1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
9f678f2f06f900afb4258288a0c2b8371f6bff592372f71bfa949c9840e6dc50
c2790070e27efbbc474e6080da1ee4222c56864eff47ebd8dfe5dfe90cdba91c
O=c1[nH]nc(Cc2ccccc2)cc1-c1ccccc1
O-[C;H0;D3;+0:1]1=[C;H0;D3;+0:2](-[c:3](:[c:4]):[c:5])-[C;H0;D3;+0:6](=[O;D1;H0:7])-[C;H0;D3;+0:8](-[c;H0;D3;+0:9](:[c:10]:[c:11]):[c:12]:[c:13])=[C;H0;D3;+0:14]-1-[C;D1;H3:15].[NH2;D1;+0:16]-[NH2;D1;+0:17]>>[C;D1;H3:15]-[c;H0;D3;+0:14]1:[c;H0;D3;+0:1](-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]):[n;H0;D2;+0:16]:[nH;D2;+0:17]:[...
null
[]
null
null
null
null
A solution of 2-(2-fluorophenyl)-3-hydroxy-4-methyl-5-(3-methoxyphenyl)-2,4-cyclopentadienone (310 mg, 1 mmol) and hydrazine (0.2 mL) in ethanol (5 mL) was heated at reflux for 30 minutes. The resulting solution was concentrated in vacuo and the residue was dissolved in dichloromethane, dried over sodium sulfate, filte...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Enol
null
C1=CCC=C1
c1ccnnc1
c1ccccc1.c1ccnnc1.c1ccccc1
HO-
C(C)O
null
null
COc1cccc(C2=C(C)C(O)=C(c3ccccc3F)C2=O)c1.NN>C(C)O>COc1cccc(-c2c(C)c(Cc3ccccc3F)n[nH]c2=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-13e9cb82d93847d4911378adc2ceb4c0
COc1cccc(C2=C(C)C(O)=C(c3ccccc3F)C2=O)c1.NNCCO>>COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCO)c2=O)c1
FC1=C(C=CC=C1)C=1C(C(=C(C1O)C)C1=CC(=CC=C1)OC)=O.OCCNN>>COC=1C=C(C=CC1)C=1C(N(N=C(C1C)CC1=C(C=CC=C1)F)CCO)=O
O[C:11]1=[C:12]([c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]2[F:19])[C:25](=[O:26])[C:8]([c:7]2[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[cH:27]2)=[C:9]1[CH3:10].[NH2:20][NH:21][CH2:22][CH2:23][OH:24]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7](-[c:8]2[c:9]([CH3:10])[c:11]([CH2:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[F:19...
COc1cccc(C2=C(C)C(O)=C(c3ccccc3F)C2=O)c1.NNCCO
COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCO)c2=O)c1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
9f678f2f06f900afb4258288a0c2b8371f6bff592372f71bfa949c9840e6dc50
c2790070e27efbbc474e6080da1ee4222c56864eff47ebd8dfe5dfe90cdba91c
O=c1[nH]nc(Cc2ccccc2)cc1-c1ccccc1
O-[C;H0;D3;+0:1]1=[C;H0;D3;+0:2](-[c:3](:[c:4]):[c:5])-[C;H0;D3;+0:6](=[O;D1;H0:7])-[C;H0;D3;+0:8](-[c;H0;D3;+0:9](:[c:10]:[c:11]):[c:12]:[c:13])=[C;H0;D3;+0:14]-1-[C;D1;H3:15].[C:16]-[C:17]-[NH;D2;+0:18]-[NH2;D1;+0:19]>>[C:16]-[C:17]-[n;H0;D3;+0:18]1:[n;H0;D2;+0:19]:[c;H0;D3;+0:1](-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]):[...
null
[]
null
null
null
null
A solution of 2-(2-fluorophenyl)-3-hydroxy-4-methyl-5-(3-methoxyphenyl)-2,4-cyclopentadienone (620 mg, 2 mmol) and hydroxylethylhydrazine (360 mg, 45 mmol)) in ethanol (5 mL) was heated at reflux for 6 hours. The resulting solution was concentrated in vacuo and the residue was dissolved in ethyl acetate (80 mL), washed...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Enol
null
C1=CCC=C1
c1ccnnc1
c1ccccc1.c1ccnnc1.c1ccccc1
HO-
C(C)O
null
null
COc1cccc(C2=C(C)C(O)=C(c3ccccc3F)C2=O)c1.NNCCO>C(C)O>COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCO)c2=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-111159e019154de4a7d6678f976321db
COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCO)c2=O)c1.NC(=O)CCC(=O)NBr>>COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCBr)c2=O)c1
COC=1C=C(C=CC1)C=1C(N(N=C(C1C)CC1=C(C=CC=C1)F)CCO)=O.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.BrNC(CCC(=O)N)=O>>COC=1C=C(C=CC1)C=1C(N(N=C(C1C)CC1=C(C=CC=C1)F)CCBr)=O
O[CH2:23][CH2:22][n:21]1[n:20][c:11]([CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]2[F:19])[c:9]([CH3:10])[c:8](-[c:7]2[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[cH:27]2)[c:25]1=[O:26].NC(=O)CCC(=O)N[Br:24]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7](-[c:8]2[c:9]([CH3:10])[c:11]([CH2:12][c:13]3[cH:14][cH:15][cH:16][cH:17]...
COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCO)c2=O)c1.NC(=O)CCC(=O)NBr
COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCBr)c2=O)c1
null
null
ClCCl
Functional Group Interconversion
OtherReaction
36d5a3000ac6c18c3e3d0fda946e9d162639e9954840bbf4cf8fd21a99f6135c
a49bb2725045f0903d387e3d995d862f3db137c208b16c8cc18a21cfd61f70da
O=c1[nH]nc(Cc2ccccc2)cc1-c1ccccc1
N-C(=O)-C-C-C(=O)-N-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3]-[#7;a:4]>>[#7;a:4]-[C:3]-[CH2;D2;+0:2]-[Br;H0;D1;+0:1]
null
[]
null
null
null
null
A solution of 4-(3-methoxyphenyl)-5-methyl-6-(2-fluorobenzyl)-2-(2-hydroxyethyl)-pyridazin-3-one (from above) and triphenylphospine (570 mg, 22 mmol) in dichloromethane (8 mL) was treated with N-bromosuccinamide (400 mg, 22 mmol) at room temperature for 2 hours. The crude product was used for next step. MS: 431 (MH+). ...
10.6084/m9.figshare.5104873.v1
null
Primary amide.Secondary amide.Primary alcohol
Primary halide
null
null
c1ccccc1.c1ccnnc1.c1ccccc1
HO-
ClCCl
null
null
COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCO)c2=O)c1.NC(=O)CCC(=O)NBr>ClCCl>COc1cccc(-c2c(C)c(Cc3ccccc3F)nn(CCBr)c2=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8b13a4b0757b40a8898d525d3471093f
CC(=O)CC(N)=O.CC(=O)CCc1ccccc1>>Cc1cc(=O)[nH]c(C)c1Cc1ccccc1
C(C)N(CC)CC.C(CC(=O)C)(=O)N.C(C1=CC=CC=C1)CC(C)=O.C(=O)(O)[O-].[Na+]>>CC1=CC(NC(=C1CC1=CC=CC=C1)C)=O
O=[C:2]([CH3:1])[CH2:3][C:4](=[O:5])[NH2:6].O=[C:7]([CH3:8])[CH2:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[CH3:1][c:2]1[cH:3][c:4](=[O:5])[nH:6][c:7]([CH3:8])[c:9]1[CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
CC(=O)CC(N)=O.CC(=O)CCc1ccccc1
Cc1cc(=O)[nH]c(C)c1Cc1ccccc1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b2102c13f169246c5fe8ffd69c8ad8da352abb9558cb6f061dbf87baa4772c09
cdc788bdba482cc2c9ffd89eee5afbfeead5621988d88b4abcccc085cefd94a3
O=c1ccc(Cc2ccccc2)c[nH]1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH2;D2;+0:3]-[C;H0;D3;+0:4](-[NH2;D1;+0:5])=[O;D1;H0:6].O=[C;H0;D3;+0:7](-[C;D1;H3:8])-[CH2;D2;+0:9]-[C:10]-[c:11]>>[C;D1;H3:2]-[c;H0;D3;+0:1]1:[cH;D2;+0:3]:[c;H0;D3;+0:4](=[O;D1;H0:6]):[nH;D2;+0:5]:[c;H0;D3;+0:7](-[C;D1;H3:8]):[c;H0;D3;+0:9]:1-[C:10]-[c:11]
53.8
[{"value": 53.8, "product": "CC1=CC(NC(=C1CC1=CC=CC=C1)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 53.7, "product": "CC1=CC(NC(=C1CC1=CC=CC=C1)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
125
CELSIUS
null
null
To a mixture of PPA (10 g) and acetoacetamide triethylamine (2.02 g, 20 mmol) was added benzylacetone (5.92 g, 5.98 mL, 40 mmol). The resulting mixture was heated at 125° C. for 3 hours. The brown mixture was poured onto crushed ice and neutralized with solid NaHCO3. The mixture was filtered to give a yellow solid, whi...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone.Primary amide
null
null
c1cccnc1
c1cccnc1.c1ccccc1
HO-
null
125
null
CC(=O)CC(N)=O.CC(=O)CCc1ccccc1>>Cc1cc(=O)[nH]c(C)c1Cc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d8e9a1700e45465cbda2d0a58ec838a6
BrBr.Cc1cc(=O)[nH]c(C)c1Cc1ccccc1>>Cc1[nH]c(=O)c(Br)c(C)c1Cc1ccccc1
N#N.CC1=CC(NC(=C1CC1=CC=CC=C1)C)=O.BrBr>>CC1=C(C(NC(=C1CC1=CC=CC=C1)C)=O)Br
Br[Br:7].[CH3:1][c:2]1[nH:3][c:4](=[O:5])[cH:6][c:8]([CH3:9])[c:10]1[CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1>>[CH3:1][c:2]1[nH:3][c:4](=[O:5])[c:6]([Br:7])[c:8]([CH3:9])[c:10]1[CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1
BrBr.Cc1cc(=O)[nH]c(C)c1Cc1ccccc1
Cc1[nH]c(=O)c(Br)c(C)c1Cc1ccccc1
null
null
C(C)(=O)O
Functional Group Interconversion
Bromination
f63fbe5668c3da6d73cce6f10b3e54926f6839a19c12cb46764f159579089aea
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
O=c1ccc(Cc2ccccc2)c[nH]1
Br-[Br;H0;D1;+0:1].[C;D1;H3:2]-[c:3]1:[c:4]:[c:5]:[#7;a:6]:[c:7](=[O;D1;H0:8]):[cH;D2;+0:9]:1>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:9]1:[c:7](=[O;D1;H0:8]):[#7;a:6]:[c:5]:[c:4]:[c:3]:1-[C;D1;H3:2]
104.3
[{"value": 100.0, "product": "CC1=C(C(NC(=C1CC1=CC=CC=C1)C)=O)Br", "details": "PERCENTYIELD", "is_desired": false}, {"value": 104.3, "product": "CC1=C(C(NC(=C1CC1=CC=CC=C1)C)=O)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 4,6-dimethyl-5-benzyl-1H-pyridin-2-one (2.21 g, 10.4 mmol) in anhydrous acetic acid (10 mL) was added bromine (3.3 g, 1.06 mL, 20.7 mL). It was stirred at room temperature for one hour. Then the reaction vessel was blew N2 to remove bromine and evaporation removed volatiles. The residue was partitioned...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1cccnc1
c1ccncc1
c1ccncc1.c1ccccc1
HBr
C(C)(=O)O
null
1
BrBr.Cc1cc(=O)[nH]c(C)c1Cc1ccccc1>C(C)(=O)O>Cc1[nH]c(=O)c(Br)c(C)c1Cc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-13068739581c41bd9f653f3721546bda
CS(=O)(=O)Cl.OC[C@H]1COc2cccnc2O1>>CS(=O)(=O)OC[C@@H]1COc2cccnc2O1
CS(=O)(=O)Cl.O1C[C@@H](OC2=NC=CC=C21)CO.C(C)N(CC)CC>>CS(=O)(=O)OC[C@@H]1COC=2C(=NC=CC2)O1
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][C@H:7]1[CH2:8][O:9][c:10]2[cH:11][cH:12][cH:13][n:14][c:15]2[O:16]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][C@@H:7]1[CH2:8][O:9][c:10]2[cH:11][cH:12][cH:13][n:14][c:15]2[O:16]1
CS(=O)(=O)Cl.OC[C@H]1COc2cccnc2O1
CS(=O)(=O)OC[C@@H]1COc2cccnc2O1
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1cnc2c(c1)OCCO2
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#8:5]-[C:6]-[C:7]-[OH;D1;+0:8]>>[#8:5]-[C:6]-[C:7]-[O;H0;D2;+0:8]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
88.6
[{"value": 88.6, "product": "CS(=O)(=O)OC[C@@H]1COC=2C(=NC=CC2)O1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
A mixture of intermediate (2-a) (0.023 mol) and triethylamine (0.046 mol) in DCM (40 ml) was stirred at 0° C. A mixure of methanesulfonyl chloride (0.035 mol) in DCM (10 ml) was added dropwise. The mixture was stirred on an ice bath for 2 hours and then washed with H2O/NaCl. The organic layer was dried, filtered and th...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1cnc2c(c1)OCCO2
HCl
C(Cl)Cl
0
null
CS(=O)(=O)Cl.OC[C@H]1COc2cccnc2O1>C(Cl)Cl>CS(=O)(=O)OC[C@@H]1COc2cccnc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-52bd9af9abde4dd88619b3dcdc6bb275
COC(=O)C1Oc2cccnc2O1>>OCC1Oc2cccnc2O1
[NH4+].[Cl-].O1C(OC2=NC=CC=C21)C(=O)OC.[H-].[H-].[H-].[H-].[Li+].[Al+3]>>O1C(OC2=NC=CC=C21)CO
CO[C:2](=[O:1])[CH:3]1[O:4][c:5]2[cH:6][cH:7][cH:8][n:9][c:10]2[O:11]1>>[OH:1][CH2:2][CH:3]1[O:4][c:5]2[cH:6][cH:7][cH:8][n:9][c:10]2[O:11]1
COC(=O)C1Oc2cccnc2O1
OCC1Oc2cccnc2O1
null
null
O.C(C)(=O)OCC.C1CCOC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1cnc2c(c1)OCO2
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]1-[#8:4]-[c:5](:[#7;a:6]):[c:7]-[#8:8]-1>>[#7;a:6]:[c:5]1:[c:7]-[#8:8]-[C:3](-[CH2;D2;+0:1]-[OH;D1;+0:2])-[#8:4]-1
43.2
[{"value": 43.2, "product": "O1C(OC2=NC=CC=C21)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
Reaction under a nitrogen atmosphere. A solution of intermediate (4) (0.042 mol) in THF (48 ml) was added dropwise to LiAlH4 (1 Min THF) (0.0466 mol) and cooled with an ice-water bath. The resulting reaction mixture was stirred for one hour at room temperature. The reaction mixture was treated carefully with a 10% NH4C...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1cnc2c(c1)OCO2
Other
O.C(C)(=O)OCC.C1CCOC1
null
1
COC(=O)C1Oc2cccnc2O1>O.C(C)(=O)OCC.C1CCOC1>OCC1Oc2cccnc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a094a34095174cc381d440ed23ac3e00
CS(=O)(=O)Cl.OCC1Oc2cccnc2O1>>CS(=O)(=O)OCC1Oc2cccnc2O1
O1C(OC2=NC=CC=C21)CO.C(C)N(CC)CC.CS(=O)(=O)Cl>>CS(=O)(=O)OCC1OC=2C(=NC=CC2)O1
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][CH:7]1[O:8][c:9]2[cH:10][cH:11][cH:12][n:13][c:14]2[O:15]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][CH:7]1[O:8][c:9]2[cH:10][cH:11][cH:12][n:13][c:14]2[O:15]1
CS(=O)(=O)Cl.OCC1Oc2cccnc2O1
CS(=O)(=O)OCC1Oc2cccnc2O1
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1cnc2c(c1)OCO2
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#8:5]-[C:6](-[C:7]-[OH;D1;+0:8])-[#8:9]>>[#8:5]-[C:6](-[C:7]-[O;H0;D2;+0:8]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4])-[#8:9]
100.9
[{"value": 100.9, "product": "CS(=O)(=O)OCC1OC=2C(=NC=CC2)O1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A solution of intermediate (5) (0.018 mol) and triethyl amine (0.036 mol) in DCM (80 ml) was stirred and cooled with an ice-water bath. Methanesulfonyl chloride (0.027 mol) was added dropwise and the resulting reaction mixture was stirred for one hour while cooling on an ice-bath. The crude reaction mixture was washed ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1cnc2c(c1)OCO2
HCl
C(Cl)Cl
null
1
CS(=O)(=O)Cl.OCC1Oc2cccnc2O1>C(Cl)Cl>CS(=O)(=O)OCC1Oc2cccnc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-55ae6d3dbf894db8b54952ca5af88cf3
C=CCO.COCOc1cnccc1Cl>>C=CCOc1ccncc1OCOC
COCOC=1C=NC=CC1Cl.C(C=C)O.[H-].[Na+]>>COCOC=1C=NC=CC1OCC=C
[CH2:1]=[CH:2][CH2:3][OH:4].Cl[c:5]1[cH:6][cH:7][n:8][cH:9][c:10]1[O:11][CH2:12][O:13][CH3:14]>>[CH2:1]=[CH:2][CH2:3][O:4][c:5]1[cH:6][cH:7][n:8][cH:9][c:10]1[O:11][CH2:12][O:13][CH3:14]
C=CCO.COCOc1cnccc1Cl
C=CCOc1ccncc1OCOC
null
null
COCCOC
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
ea617b323b892eda23f5ae30e789991ea9692064ef355a16e8ed81c16e743d2b
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1ccncc1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5]:[c:6]:1-[#8:7].[C;D1;H2:8]=[C:9]-[C:10]-[OH;D1;+0:11]>>[#8:7]-[c:6]1:[c:5]:[#7;a:4]:[c:3]:[c:2]:[c;H0;D3;+0:1]:1-[O;H0;D2;+0:11]-[C:10]-[C:9]=[C;D1;H2:8]
54.2
[{"value": 54.2, "product": "COCOC=1C=NC=CC1OCC=C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
Under nitrogen atmosphere. 2-propen-1-ol (0.002 mol) was added dropwise to a stirred mixture of NaH 60% (0.002 mol) in DME (5ml). The mixture was stirred at room temperature for 15 minutes. A solution of 3-(methoxymethoxy)-4-chloropyridine (0.0017 mol) in DME (5 ml) was added dropwise. The resulting reaction mixture wa...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1ccncc1
c1ccncc1
c1ccncc1
HCl
COCCOC
null
0.25
C=CCO.COCOc1cnccc1Cl>COCCOC>C=CCOc1ccncc1OCOC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8fb04d6901e243ce83f9b846bd236967
COCOc1cnccc1OCC(Br)CBr>>Oc1cnccc1OCC(Br)CBr
BrC(COC1=C(C=NC=C1)OCOC)CBr.Cl>>BrC(COC1=C(C=NC=C1)O)CBr
COC[O:1][c:2]1[cH:3][n:4][cH:5][cH:6][c:7]1[O:8][CH2:9][CH:10]([Br:11])[CH2:12][Br:13]>>[OH:1][c:2]1[cH:3][n:4][cH:5][cH:6][c:7]1[O:8][CH2:9][CH:10]([Br:11])[CH2:12][Br:13]
COCOc1cnccc1OCC(Br)CBr
Oc1cnccc1OCC(Br)CBr
null
null
C(C)O
Reduction
OtherReaction
92f30feec6876d2f8c7439342f0f488fd5811a8fdb3b3cb63d7289bd57242715
3165f563067f8d27bb50b0da034e3e854d1ead7f745de7cf575f7ca4cf677789
c1ccncc1
C-O-C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
55.4
[{"value": 55.4, "product": "BrC(COC1=C(C=NC=C1)O)CBr", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A mixture of intermediate (8) (0.0248 mol), HCl (35.42 ml)and ethanol (40 ml) was stirred at room temperature overnight. The reaction mixture was concentrated under vacuum. The concentrate was cooled on an ice-water bath. The mixture was neutralized with a saturated NaHCO3 solution and extracted with ethyl acetate. The...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Aromatic alcohol
null
null
c1ccncc1
HO-
C(C)O
null
8
COCOc1cnccc1OCC(Br)CBr>C(C)O>Oc1cnccc1OCC(Br)CBr
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4a1d3a61ac65482faaad1b568ca78b0e
Oc1cnccc1OCC(Br)CBr>>BrCC1COc2ccncc2O1
BrC(COC1=C(C=NC=C1)O)CBr.C(=O)(O)[O-].[Na+]>>BrCC1COC2=C(C=NC=C2)O1
Br[CH:3]([CH2:2][Br:1])[CH2:4][O:5][c:6]1[cH:7][cH:8][n:9][cH:10][c:11]1[OH:12]>>[Br:1][CH2:2][CH:3]1[CH2:4][O:5][c:6]2[cH:7][cH:8][n:9][cH:10][c:11]2[O:12]1
Oc1cnccc1OCC(Br)CBr
BrCC1COc2ccncc2O1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
f4643c98d3fbb3e020f3059aacbfe64fa7986154641510e15c8b2587fd92d396
cf768afb66ed5041aefdce1fa6d1e40995a1ab7c4b4a4ca47544fe49ee1e629f
c1cc2c(cn1)OCCO2
Br-[CH;D3;+0:1](-[C:2]-[Br;D1;H0:3])-[C:4]-[#8:5]-[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[#7;a:10]:[c:11]>>[Br;D1;H0:3]-[C:2]-[CH;D3;+0:1]1-[C:4]-[#8:5]-[c:6]:[c:7](:[c:9]:[#7;a:10]:[c:11])-[O;H0;D2;+0:8]-1
67.7
[{"value": 67.7, "product": "BrCC1COC2=C(C=NC=C2)O1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of intermediate (9) (0.0097 mol) in ethanol (50 ml) was stirred and refluxed overnight. NaHCO3 (0.0097 mol) was added and the resulting reaction mixture was stirred and refluxed overnight. The solvent was evaporated. The residue was washed with water and extracted with DCM. The organic layer was dried, filte...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Aromatic alcohol
Ether
null
c1cc2c(cn1)OCCO2
c1cc2c(cn1)OCCO2
HBr
C(C)O
null
null
Oc1cnccc1OCC(Br)CBr>C(C)O>BrCC1COc2ccncc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2579d2b9ed544c63b1824890ac07c44c
C=CC#N.CC(C)(CN)CN>>CC(C)(CN)CNCCC#N
CC(CN)(CN)C.C(C=C)#N.CC(CN)(CN)C.C(C=C)#N>>NCC(CNCCC#N)(C)C
[CH2:8]=[CH:9][C:10]#[N:11].[CH3:1][C:2]([CH3:3])([CH2:4][NH2:5])[CH2:6][NH2:7]>>[CH3:1][C:2]([CH3:3])([CH2:4][NH2:5])[CH2:6][NH:7][CH2:8][CH2:9][C:10]#[N:11]
C=CC#N.CC(C)(CN)CN
CC(C)(CN)CNCCC#N
null
null
C(C)O
Heteroatom Alkylation and Arylation
aza-Michael addition primary
b45dd075b7e75caee6dc0a68cb402266c75e0848f7502f06a5dbd8a34863aae2
2e45960e6468a140db4162555f247a2535630c23e1aa16e082b84ce22691ebbf
null
[CH2;D1;+0:1]=[CH;D2;+0:2]-[C:3]#[N;D1;H0:4].[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:5]-[C:6]-[NH;D2;+0:7]-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[C:3]#[N;D1;H0:4]
79.6
[{"value": 79.6, "product": "NCC(CNCCC#N)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A mixture of 2,2 dimethyl-1,3-propanediamine (0.22 mol) and 2-propenenitrile (0.22 mol) in ethanol (250 ml) was stirred overnight at room temperature. The solvent was evaporated. A mixture of 2,2-dimethyl-1,3-propanediamine (0.28 mol) and 2-propenenitrile (0.28 mol) in ethanol (250 ml) was stirred for one hour at room ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Vinyl
Secondary amine
null
null
null
null
C(C)O
null
8
C=CC#N.CC(C)(CN)CN>C(C)O>CC(C)(CN)CNCCC#N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9d4167a8912c427091dedcf06cd80dc8
C=CC#N.NC1(CO)CCN(Cc2ccccc2)CC1>>N#CCCNC1(CO)CCN(Cc2ccccc2)CC1
C(C=C)#N.NC1(CCN(CC1)CC1=CC=CC=C1)CO.C(C=C)#N.C(C=C)#N>>OCC1(CCN(CC1)CC1=CC=CC=C1)NCCC#N
[N:1]#[C:2][CH:3]=[CH2:4].[NH2:5][C:6]1([CH2:7][OH:8])[CH2:9][CH2:10][N:11]([CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[CH2:19][CH2:20]1>>[N:1]#[C:2][CH2:3][CH2:4][NH:5][C:6]1([CH2:7][OH:8])[CH2:9][CH2:10][N:11]([CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[CH2:19][CH2:20]1
C=CC#N.NC1(CO)CCN(Cc2ccccc2)CC1
N#CCCNC1(CO)CCN(Cc2ccccc2)CC1
null
null
C(C)O
Heteroatom Alkylation and Arylation
aza-Michael addition primary
b45dd075b7e75caee6dc0a68cb402266c75e0848f7502f06a5dbd8a34863aae2
2e45960e6468a140db4162555f247a2535630c23e1aa16e082b84ce22691ebbf
c1ccc(CN2CCCCC2)cc1
[CH2;D1;+0:1]=[CH;D2;+0:2]-[C:3]#[N;D1;H0:4].[C:5]-[C:6](-[C:7])(-[NH2;D1;+0:8])-[C:9]>>[C:5]-[C:6](-[C:7])(-[NH;D2;+0:8]-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[C:3]#[N;D1;H0:4])-[C:9]
null
[]
null
null
null
null
A mixture of 4-amino-1-(phenylmethyl)-4-piperidinemethanol (0.0182 mol) and 2-propenenitrile (0.0304 mol) in ethanol (80 ml) was stirred and refluxed for two days. 2-Propenenitrile (2 ml) was added. The mixture was stirred and refluxed for 5 hours. 2-Propenenitrile (2 ml) was added again. The mixture was stirred and re...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Vinyl
Secondary amine
null
null
C1CC[NH]CC1.c1ccccc1
null
C(C)O
null
null
C=CC#N.NC1(CO)CCN(Cc2ccccc2)CC1>C(C)O>N#CCCNC1(CO)CCN(Cc2ccccc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-46e7da05dc1e4904ba0a0abab488250d
N#CCCNC1(CO)CCN(Cc2ccccc2)CC1>>NCCCNC1(CO)CCN(Cc2ccccc2)CC1
[H][H].OCC1(CCN(CC1)CC1=CC=CC=C1)NCCC#N.N>>NCCCNC1(CCN(CC1)CC1=CC=CC=C1)CO
[N:1]#[C:2][CH2:3][CH2:4][NH:5][C:6]1([CH2:7][OH:8])[CH2:9][CH2:10][N:11]([CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[CH2:19][CH2:20]1>>[NH2:1][CH2:2][CH2:3][CH2:4][NH:5][C:6]1([CH2:7][OH:8])[CH2:9][CH2:10][N:11]([CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[CH2:19][CH2:20]1
N#CCCNC1(CO)CCN(Cc2ccccc2)CC1
NCCCNC1(CO)CCN(Cc2ccccc2)CC1
null
[Ni]
CO
Reduction
Reduction of nitrile to amine
65bec2d9f430701d30dc9fcbe1c5418f3dfa174d67be035c50edfc71895dc9c7
e8d1bc928b94bd4f5bf4b23363ce8f88b1ce7d146ba93829e7b8ad8dbe0007a7
c1ccc(CN2CCCCC2)cc1
[C:1]-[C:2]-[C;H0;D2;+0:3]#[N;H0;D1;+0:4]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[NH2;D1;+0:4]
86.2
[{"value": 86.2, "product": "NCCCNC1(CCN(CC1)CC1=CC=CC=C1)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of intermediate (14) (0.0159 mol) in methanol saturated with NH3 (150 ml) was hydrogenated at 14° C. with Raney nickel (½ spoon) as a catalyst. After uptake of hydrogen (2 equivalents), the catalyst was filtered off and the filtrate was evaporated, yielding 3.8 g of 4-[(3-aminopropyl)amino]-1-(phenylmethyl)-4...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
C1CC[NH]CC1.c1ccccc1
null
[Ni].CO
null
null
N#CCCNC1(CO)CCN(Cc2ccccc2)CC1>[Ni].CO>NCCCNC1(CO)CCN(Cc2ccccc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e31df8ebcd91409b97b45604f0093f7e
NCCCNC1(CO)CCN(Cc2ccccc2)CC1.O=C(n1ccnc1)n1ccnc1>>O=C1NCCCN1C1(CO)CCN(Cc2ccccc2)CC1
C(=O)(N1C=NC=C1)N1C=NC=C1.NCCCNC1(CCN(CC1)CC1=CC=CC=C1)CO>>OCC1(CCN(CC1)CC1=CC=CC=C1)N1C(NCCC1)=O
[NH2:3][CH2:4][CH2:5][CH2:6][NH:7][C:8]1([CH2:9][OH:10])[CH2:11][CH2:12][N:13]([CH2:14][c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[CH2:21][CH2:22]1.c1cn([C:2](n2ccnc2)=[O:1])cn1>>[O:1]=[C:2]1[NH:3][CH2:4][CH2:5][CH2:6][N:7]1[C:8]1([CH2:9][OH:10])[CH2:11][CH2:12][N:13]([CH2:14][c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]...
NCCCNC1(CO)CCN(Cc2ccccc2)CC1.O=C(n1ccnc1)n1ccnc1
O=C1NCCCN1C1(CO)CCN(Cc2ccccc2)CC1
null
null
C1CCOC1
Acylation
OtherReaction
57b05020c91f5cbcbf12dad7925c21eec46f26a456a38df2d6da259ef3d4778c
092fb1988ce3c31a0210cc9ec123f317c79841c29a05a3f2098134944f12c379
O=C1NCCCN1C1CCN(Cc2ccccc2)CC1
[C:1]-[C:2](-[C:3])(-[NH;D2;+0:4]-[C:5]-[C:6]-[C:7]-[NH2;D1;+0:8])-[C:9].[O;D1;H0:10]=[C;H0;D3;+0:11](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[C:1]-[C:2](-[C:3])(-[N;H0;D3;+0:4]1-[C:5]-[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:11]-1=[O;D1;H0:10])-[C:9]
49.3
[{"value": 49.3, "product": "OCC1(CCN(CC1)CC1=CC=CC=C1)N1C(NCCC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
1,1′-Carbonylbis-1H-imidazole (0.0149 mol) was added to a mixture of intermediate (15) (0.0137 mol) in THF (40 ml). The mixture was stirred at room temperature overnight. The precipitate was filtered off, crystallized from ACN, filtered off, washed with ACN and DIPE and then dried, yielding 2.05 g of tetrahydro-1-[4-(h...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Secondary amine
Urea
c1c[nH]cn1.c1c[nH]cn1
C1CNC[NH]C1
C1CNC[NH]C1.C1CC[NH]CC1.c1ccccc1
Other
C1CCOC1
null
8
NCCCNC1(CO)CCN(Cc2ccccc2)CC1.O=C(n1ccnc1)n1ccnc1>C1CCOC1>O=C1NCCCN1C1(CO)CCN(Cc2ccccc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a22ad81d826e47c9accc03b29bb160d2
O=C1NCCCN1C1(CO)CCN(Cc2ccccc2)CC1>>O=C1NCCCN1C1(CO)CCNCC1
OCC1(CCN(CC1)CC1=CC=CC=C1)N1C(NCCC1)=O.[H][H]>>OCC1(CCNCC1)N1C(NCCC1)=O
c1ccc(C[N:13]2[CH2:12][CH2:11][C:8]([N:7]3[C:2](=[O:1])[NH:3][CH2:4][CH2:5][CH2:6]3)([CH2:9][OH:10])[CH2:15][CH2:14]2)cc1>>[O:1]=[C:2]1[NH:3][CH2:4][CH2:5][CH2:6][N:7]1[C:8]1([CH2:9][OH:10])[CH2:11][CH2:12][NH:13][CH2:14][CH2:15]1
O=C1NCCCN1C1(CO)CCN(Cc2ccccc2)CC1
O=C1NCCCN1C1(CO)CCNCC1
null
[Pd]
CO
Deprotection
Hydrogenolysis of tertiary amines
cd3c1aa319cad45f383f17cc0b8bfc8337d7078d779f654933f9a447e64292a5
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
O=C1NCCCN1C1CCNCC1
[C:1]-[C:2]-[N;H0;D3;+0:3](-C-c1:c:c:c:c:c:1)-[C:4]-[C:5]>>[C:1]-[C:2]-[NH;D2;+0:3]-[C:4]-[C:5]
47.7
[{"value": 47.7, "product": "OCC1(CCNCC1)N1C(NCCC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of intermediate (16) (0.0059 mol) in methanol (100 ml) was hydrogenated with palladium on carbon (1 g) as a catalyst. After uptake of hydrogen (1 equivalent), the catalyst was filtered off, the filtrate was evaporated and crystallized from ACN, yielding 0.6 g of tetrahydro-1-[4(hydroxymethyl)-4-piperidinyl]-2...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.C1CC[NH]CC1
C1CCNCC1
C1CNC[NH]C1.C1CCNCC1
Other
[Pd].CO
null
null
O=C1NCCCN1C1(CO)CCN(Cc2ccccc2)CC1>[Pd].CO>O=C1NCCCN1C1(CO)CCNCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a9967f9e01b644cebaf2b22cfd6b0467
C=CCN1CC(=O)NC1=O>>O=C1CN(CC2CO2)C(=O)N1
C(=O)([O-])[O-].[Na+].[Na+].C(C=C)N1C(NC(C1)=O)=O.ClC=1C=C(C=CC1)C(=O)OO.S([O-])(O)=O>>O1C(C1)CN1C(NC(C1)=O)=O
[O:1]=[C:2]1[CH2:3][N:4]([CH2:5][CH:6]=[CH2:7])[C:9](=[O:10])[NH:11]1>>[O:1]=[C:2]1[CH2:3][N:4]([CH2:5][CH:6]2[CH2:7][O:8]2)[C:9](=[O:10])[NH:11]1
C=CCN1CC(=O)NC1=O
O=C1CN(CC2CO2)C(=O)N1
null
null
C(Cl)Cl
Oxidation
OtherReaction
ccc410867e4c89598d5079c0dfc27f7bc863046b1c1459e93fa3815bf371d797
38c38e5e943ba321612c1e8763ee5b6d3bec0e5b922509df80b788fc9703980f
O=C1CN(CC2CO2)C(=O)N1
[CH2;D1;+0:1]=[CH;D2;+0:2]-[C:3]-[#7:4]-[C:5]=[O;D1;H0:6]>>[O;D1;H0:6]=[C:5]-[#7:4]-[C:3]-[CH;D3;+0:2]1-[#8:7]-[CH2;D2;+0:1]-1
89
[{"value": 89.0, "product": "O1C(C1)CN1C(NC(C1)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
A reaction solution of 1-(2-propenyl)-2,4-imidazolidinedione (0.036 mol) and 3-chloro-benzenecarboperoxoic acid (0.043 mol, 70.75%) in DCM (25 ml) was stirred for 2 hours at room temperature. An aqueous solution of bisulfite was added and the mixture was stirred for 10 minutes. Na2CO3 was added and this mixture was ext...
10.6084/m9.figshare.5104873.v1
null
Allyl
Ether
null
C1CO1
C1C[NH]CN1.C1CO1
Other
C(Cl)Cl
null
0.166667
C=CCN1CC(=O)NC1=O>C(Cl)Cl>O=C1CN(CC2CO2)C(=O)N1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d050e9c621754d0090d82aad60627c10
ClCC1CO1.Oc1cccnc1Cl>>Clc1ncccc1OCC1CO1
O.ClCC1OC1.Cl.ClC1=NC=CC=C1O.[H-].[Na+]>>ClC1=NC=CC=C1OCC1OC1
Cl[CH2:9][CH:10]1[CH2:11][O:12]1.[Cl:1][c:2]1[n:3][cH:4][cH:5][cH:6][c:7]1[OH:8]>>[Cl:1][c:2]1[n:3][cH:4][cH:5][cH:6][c:7]1[O:8][CH2:9][CH:10]1[CH2:11][O:12]1
ClCC1CO1.Oc1cccnc1Cl
Clc1ncccc1OCC1CO1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1cncc(OCC2CO2)c1
Cl-[CH2;D2;+0:1]-[C:2]1-[#8:3]-[C:4]-1.[Cl;D1;H0:5]-[c:6](:[#7;a:7]:[c:8]):[c:9](-[OH;D1;+0:10]):[c:11]>>[Cl;D1;H0:5]-[c:6](:[#7;a:7]:[c:8]):[c:9](-[O;H0;D2;+0:10]-[CH2;D2;+0:1]-[C:2]1-[#8:3]-[C:4]-1):[c:11]
194.4
[{"value": 194.4, "product": "ClC1=NC=CC=C1OCC1OC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Reaction was carried out under nitrogen flow. A mixture of 2-chloro-3-pyridinol hydrochloride (1:1) (1.760 mol) in DMF (1000 ml) was added dropwise in 30 minutes to a mixture of NaH 60% (1.934 mol) in DMF (1200 ml) (temperature below 27° C.). The reaction mixture was stirred for 30 minutes. (Chloromethyl)-oxirane (3.53...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccncc1.C1CO1
HCl
CN(C)C=O
null
0.5
ClCC1CO1.Oc1cccnc1Cl>CN(C)C=O>Clc1ncccc1OCC1CO1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f0951644cba643059e43008a1e0b23cf
Clc1ncccc1OCC1CO1.OCc1ccccc1>>C=C/C=C\CCOCC(O)COc1cccnc1Cl
ClC1=NC=CC=C1OCC1OC1.C1CCOC1.C1(=CC=CC=C1)CO.[OH-].[Na+]>>ClC1=NC=CC=C1OCC(COCC\C=C/C=C)O
[CH2:8]1[CH:9]([CH2:11][O:12][c:13]2[cH:14][cH:15][cH:16][n:17][c:18]2[Cl:19])[O:10]1.c1[cH:1][cH:2][cH:3][cH:4][c:5]1[CH2:6][OH:7]>>[CH2:1]=[CH:2]/[CH:3]=[CH:4]\[CH2:5][CH2:6][O:7][CH2:8][CH:9]([OH:10])[CH2:11][O:12][c:13]1[cH:14][cH:15][cH:16][n:17][c:18]1[Cl:19]
Clc1ncccc1OCC1CO1.OCc1ccccc1
C=C/C=C\CCOCC(O)COc1cccnc1Cl
null
null
O
Functional Group Interconversion
OtherReaction
08d986e85e248a77573253bc1bd35c6979479678e0e5c2c4618bb6cac4dbaec1
1eaac4c438ebea37734abc461df3eafd66a8a51fd24d58b9a1b5b047bf2c6ff8
c1ccncc1
[C:1]-[C:2]1-[CH2;D2;+0:3]-[O;H0;D2;+0:4]-1.[OH;D1;+0:5]-[C:6]-[c;H0;D3;+0:7]1:[cH;D2;+0:8]:[cH;D2;+0:9]:[cH;D2;+0:10]:[cH;D2;+0:11]:c:1>>[C:1]-[C:2](-[OH;D1;+0:4])-[CH2;D2;+0:3]-[O;H0;D2;+0:5]-[C:6]-[CH2;D2;+0:7]/[CH;D2;+0:8]=[CH;D2;+0:9]\[CH;D2;+0:10]=[CH2;D1;+0:11]
38
[{"value": 38.0, "product": "ClC1=NC=CC=C1OCC(COCC\\C=C/C=C)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A mixture of THF (915 ml), benzenemethanol (2.96 mol) and NaOH (2.36 mol) was stirred at room temperature for 30 minutes (cooling was required to keep the temperature below 25° C.). Intermediate (19) (1.97 mol) was added. The reaction mixture was stirred at room temperature for 4 days. Water was added dropwise (cooling...
10.6084/m9.figshare.5104873.v1
null
Ether.Primary alcohol
Ether.Secondary alcohol.Vinyl.Conjugated diene
C1CO1.c1ccccc1
null
c1ccncc1
Other
O
null
0.5
Clc1ncccc1OCC1CO1.OCc1ccccc1>O>C=C/C=C\CCOCC(O)COc1cccnc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e863c07b645248fda8f4ffad40dc7b47
C=C(C(=O)O)P(=O)(OCC)OCC.O=Cc1ncccc1O>>CCOC(=O)C1=Cc2ncccc2OC1
[NH4+].[Cl-].C(C)OP(=O)(C(C(=O)O)=C)OCC.C1CCOC1.[H-].[Na+].C1CCOC1.OC=1C(=NC=CC1)C=O.C1CCOC1>>O1CC(=CC2=NC=CC=C21)C(=O)OCC
CCOP(=O)(O[CH2:2][CH3:1])[C:6]([C:4]([OH:3])=[O:5])=[CH2:15].O=[CH:7][c:8]1[n:9][cH:10][cH:11][cH:12][c:13]1[OH:14]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]1=[CH:7][c:8]2[n:9][cH:10][cH:11][cH:12][c:13]2[O:14][CH2:15]1
C=C(C(=O)O)P(=O)(OCC)OCC.O=Cc1ncccc1O
CCOC(=O)C1=Cc2ncccc2OC1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
c35822cd68bf53c853ab7a1ede5bfc04d46a9c76cf1d473da361362721f47599
fc2575a0b5bf17c182baee9326f66494e91d02a86703b6684cb158a39ed47b67
C1=Cc2ncccc2OC1
C-C-O-P(=O)(-O-[CH2;D2;+0:1]-[C;D1;H3:2])-[C;H0;D3;+0:3](=[CH2;D1;+0:4])-[C:5](=[O;D1;H0:6])-[OH;D1;+0:7].O=[CH;D2;+0:8]-[c:9](:[#7;a:10]:[c:11]):[c:12](-[OH;D1;+0:13]):[c:14]>>[C;D1;H3:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:7]-[C:5](=[O;D1;H0:6])-[C;H0;D3;+0:3]1=[CH;D2;+0:8]-[c:9](:[#7;a:10]:[c:11]):[c:12](:[c:14])-[O;H0;D2;+0:...
null
[]
0
CELSIUS
null
null
A mixture of NaH 60% (0.051 mol) in THF (20 ml) was stirred at 0° C. A solution of 3-hydroxy-2-pyridinecarboxaldehyde (0.034 mol) in THF (75 ml) was added dropwise at 0° C. The reaction mixture was stirred for one hour at room temperature. A solution of 2-(diethoxyphosphinyl)-2-propenoic acid, ethyl esther (0.041 mol) ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Carboxylic acid.Aromatic alcohol.Vinyl
Ester.Ether
null
C1=Cc2ncccc2OC1
C1=Cc2ncccc2OC1
HO-
null
0
null
C=C(C(=O)O)P(=O)(OCC)OCC.O=Cc1ncccc1O>>CCOC(=O)C1=Cc2ncccc2OC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-495ba84ac0e447cda9911ec26109657e
CCOC(=O)C1=Cc2ncccc2OC1>>OCC1=Cc2ncccc2OC1
O1CC(=CC2=NC=CC=C21)C(=O)OCC.[BH4-].[Na+].[NH4+].[Cl-]>>O1CC(=CC2=NC=CC=C21)CO
CCO[C:2](=[O:1])[C:3]1=[CH:4][c:5]2[n:6][cH:7][cH:8][cH:9][c:10]2[O:11][CH2:12]1>>[OH:1][CH2:2][C:3]1=[CH:4][c:5]2[n:6][cH:7][cH:8][cH:9][c:10]2[O:11][CH2:12]1
CCOC(=O)C1=Cc2ncccc2OC1
OCC1=Cc2ncccc2OC1
null
null
CO.C1CCOC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
C1=Cc2ncccc2OC1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3](=[C:4]-[c:5]:[#7;a:6])-[C:7]-[#8:8]>>[#7;a:6]:[c:5]-[C:4]=[C:3](-[CH2;D2;+0:1]-[OH;D1;+0:2])-[C:7]-[#8:8]
86.2
[{"value": 86.2, "product": "O1CC(=CC2=NC=CC=C21)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
A solution of intermediate (24) (0.0032 mol) in methanol (dry) (2 ml) and THF (dry) (16 ml) was stirred at 0° C. NaBH4 (0.0128 mol) was added portionwise at 0° C. The reaction mixture was stirred for 5 hours at room temperature. A 10% NH4Cl solution was added and this mixture was extracted with DCM. The separated organ...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
C1=Cc2ncccc2OC1
HO-
CO.C1CCOC1
null
5
CCOC(=O)C1=Cc2ncccc2OC1>CO.C1CCOC1>OCC1=Cc2ncccc2OC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b9cbd20a7d6a4baf8ad5eba19664bb6d
OCC1=Cc2ncccc2OC1>>OCC1COc2cccnc2C1
O1CC(=CC2=NC=CC=C21)CO.[H][H]>>O1CC(CC2=NC=CC=C21)CO
[OH:1][CH2:2][C:3]1=[CH:12][c:11]2[c:6]([cH:7][cH:8][cH:9][n:10]2)[O:5][CH2:4]1>>[OH:1][CH2:2][CH:3]1[CH2:4][O:5][c:6]2[cH:7][cH:8][cH:9][n:10][c:11]2[CH2:12]1
OCC1=Cc2ncccc2OC1
OCC1COc2cccnc2C1
null
[Pd]
CO
Reduction
Hydrogenation (double to single)
7e489a1fe2ccc21e0d6c692bcb91866ae4946e46ebedca2097faddc137287202
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1cnc2c(c1)OCCC2
[O;D1;H1:1]-[C:2]-[C;H0;D3;+0:3]1=[CH;D2;+0:4]-[c:5](:[#7;a:6]:[c:7]):[c:8]-[#8:9]-[C:10]-1>>[O;D1;H1:1]-[C:2]-[CH;D3;+0:3]1-[C:10]-[#8:9]-[c:8]:[c:5](:[#7;a:6]:[c:7])-[CH2;D2;+0:4]-1
78.5
[{"value": 78.5, "product": "O1CC(CC2=NC=CC=C21)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of intermediate (25) (0.0027 mol) in methanol (20 ml) was hydrogenated for 24 hours at room temperature with palladium-on-carbon (0.04 g) as a catalyst. After uptake of hydrogen (1 equivalent), the catalyst was filtered off and the filtrate was evaporated, yielding 0.35 g of 3,4-dihydro-2H-pyrano[3,2-b]pyridi...
10.6084/m9.figshare.5104873.v1
null
null
null
C1=Cc2ncccc2OC1
c1cnc2c(c1)OCCC2
c1cnc2c(c1)OCCC2
null
[Pd].CO
null
null
OCC1=Cc2ncccc2OC1>[Pd].CO>OCC1COc2cccnc2C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f2532a0bdbb646dd95616279880e1369
CI.Nc1cccnc1Cl>>CNc1cccnc1Cl
[NH4+].[Cl-].IC.ClC1=NC=CC=C1N.C(C)(C)NC(C)C.[Li]>>ClC1=NC=CC=C1NC
I[CH3:1].[NH2:2][c:3]1[cH:4][cH:5][cH:6][n:7][c:8]1[Cl:9]>>[CH3:1][NH:2][c:3]1[cH:4][cH:5][cH:6][n:7][c:8]1[Cl:9]
CI.Nc1cccnc1Cl
CNc1cccnc1Cl
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
3c2788b3f372b76c1d2ee0d77963cb247b210aa8a28e76637b4e731826c4252a
c6874c6af41d3b1c4f7668e1cd342c90252d0e77f4317d31b3193ebc2f9501a3
c1ccncc1
I-[CH3;D1;+0:1].[Cl;D1;H0:2]-[c:3](:[#7;a:4]:[c:5]):[c:6](-[NH2;D1;+0:7]):[c:8]>>[CH3;D1;+0:1]-[NH;D2;+0:7]-[c:6](:[c:8]):[c:3](-[Cl;D1;H0:2]):[#7;a:4]:[c:5]
89.1
[{"value": 89.1, "product": "ClC1=NC=CC=C1NC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
To a solution of 2-chloro-3-pyridinamine (0.0465 mol) in THF (45ml) at −78° C. under N2 flow, lithium diisopropylamine (0.0513 mol, 2 M) was added dropwise. The mixture was allowed to warm to 0° C. and was stirred for 1 hour and then cooled to −78° C. Then iodomethane (0.0582 mol) was added and the reaction mixture was...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Secondary amine
null
null
c1ccncc1
HI
C1CCOC1
0
1
CI.Nc1cccnc1Cl>C1CCOC1>CNc1cccnc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1e3bc0647e1c48d681068c3311f015d4
CNc1cccnc1Cl.c1ccc(COCC2CO2)cc1>>OC(CNCc1cccnc1Cl)COCc1ccccc1
[NH4+].[Cl-].C1(=CC=CC=C1)COCC1OC1.ClC1=NC=CC=C1NC.C(C)(C)NC(C)C.[Li]>>ClC1=NC=CC=C1CNCC(COCC1=CC=CC=C1)O
[NH:4]([CH3:5])[c:6]1[cH:7][cH:8][cH:9][n:10][c:11]1[Cl:12].[O:1]1[CH:2]([CH2:13][O:14][CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:3]1>>[OH:1][CH:2]([CH2:3][NH:4][CH2:5][c:6]1[cH:7][cH:8][cH:9][n:10][c:11]1[Cl:12])[CH2:13][O:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1
CNc1cccnc1Cl.c1ccc(COCC2CO2)cc1
OC(CNCc1cccnc1Cl)COCc1ccccc1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
d439f7e645ce89319ce55258a32a80ac87a862ac0dde93b154e64323356ee2ea
44f0f98267935086e7e06becbfd88bd9220317f0f521b960be901561fa43c70b
c1ccc(COCCCNCc2cccnc2)cc1
[CH3;D1;+0:1]-[NH;D2;+0:2]-[c;H0;D3;+0:3]1:[c:4]:[c:5]:[c:6]:[#7;a:7]:[c:8]:1-[Cl;D1;H0:9].[C:10]-[C:11]1-[CH2;D2;+0:12]-[O;H0;D2;+0:13]-1>>[C:10]-[C:11](-[OH;D1;+0:13])-[CH2;D2;+0:12]-[NH;D2;+0:2]-[CH2;D2;+0:1]-[c;H0;D3;+0:3]1:[c:4]:[c:5]:[c:6]:[#7;a:7]:[c:8]:1-[Cl;D1;H0:9]
75.5
[{"value": 75.5, "product": "ClC1=NC=CC=C1CNCC(COCC1=CC=CC=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
To a solution of intermediate (28) (0.031 mol) in THF (50 ml) under nitrogen flow at −78° C., lithium diisopropylamine (0.062 mol, 2 M) was slowly added. The reaction mixture was allowed to warm to 0° C. and was stirred for 1 hour. After cooling again to −78° C., a solution of [(phenylmethoxy)methyl]-oxirane (0.034 mol...
10.6084/m9.figshare.5104873.v1
null
Ether.Secondary amine
Secondary alcohol.Secondary amine
c1ccncc1.C1CO1
c1ccncc1
c1ccncc1.c1ccccc1
null
C1CCOC1
0
1
CNc1cccnc1Cl.c1ccc(COCC2CO2)cc1>C1CCOC1>OC(CNCc1cccnc1Cl)COCc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7c434df8182b48b2920976e739a5bf0b
BrBr.OCC1COc2cccnc2O1>>OCC1COc2cc(Br)cnc2O1
BrBr.O1CC(OC2=NC=CC=C21)CO.BrBr>>BrC=1C=C2C(=NC1)OC(CO2)CO
Br[Br:9].[OH:1][CH2:2][CH:3]1[CH2:4][O:5][c:6]2[cH:7][cH:8][cH:10][n:11][c:12]2[O:13]1>>[OH:1][CH2:2][CH:3]1[CH2:4][O:5][c:6]2[cH:7][c:8]([Br:9])[cH:10][n:11][c:12]2[O:13]1
BrBr.OCC1COc2cccnc2O1
OCC1COc2cc(Br)cnc2O1
null
[O-]S(=O)[O-].[Na+].[Na+]
C(=O)([O-])[O-].[Na+].[Na+].C(Cl)Cl
Functional Group Interconversion
Bromination
53ae098687f59589f7887546d68b8bc2c24e46ec8e7e4682e59ffddd63bb8698
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1cnc2c(c1)OCCO2
Br-[Br;H0;D1;+0:1].[#8:2]-[c:3]1:[#7;a:4]:[c:5]:[cH;D2;+0:6]:[c:7]:[c:8]:1-[#8:9]>>[#8:2]-[c:3]1:[#7;a:4]:[c:5]:[c;H0;D3;+0:6](-[Br;H0;D1;+0:1]):[c:7]:[c:8]:1-[#8:9]
40.6
[{"value": 40.6, "product": "BrC=1C=C2C(=NC1)OC(CO2)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Bromine (0.009 mol) was added dropwise to a solution of 2,3-dihydro-1,4-dioxino[2,3-b]pyridine-3-methanol (0.009 mol) in DCM (100 ml) and Na2CO3 saturated solution (50 ml), stirred at room temperature. The reaction mixture was stirred for 16 hours at room temperature. More bromine (0.009 mol) was added and the reaction...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1cnc2c(c1)OCCO2
c1cnc2c(c1)OCCO2
c1cnc2c(c1)OCCO2
HBr
[O-]S(=O)[O-].[Na+].[Na+].C(=O)([O-])[O-].[Na+].[Na+].C(Cl)Cl
null
null
BrBr.OCC1COc2cccnc2O1>[O-]S(=O)[O-].[Na+].[Na+].C(=O)([O-])[O-].[Na+].[Na+].C(Cl)Cl>OCC1COc2cc(Br)cnc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-47a5080b79c24614836794070a39ff48
CC(C)(C)[Si](C)(C)OCC1COc2cc(Br)cnc2O1.CI>>Cc1cnc2c(c1)OCC(CO[Si](C)(C)C(C)(C)C)O2
[NH4+].[Cl-].[Li]CCCC.BrC=1C=C2C(=NC1)OC(CO2)CO[Si](C)(C)C(C)(C)C.IC>>CC(C)(C)[Si](OCC1COC=2C(=NC=C(C2)C)O1)(C)C
Br[c:2]1[cH:3][n:4][c:5]2[c:6]([cH:7]1)[O:8][CH2:9][CH:10]([CH2:11][O:12][Si:13]([CH3:14])([CH3:15])[C:16]([CH3:17])([CH3:18])[CH3:19])[O:20]2.I[CH3:1]>>[CH3:1][c:2]1[cH:3][n:4][c:5]2[c:6]([cH:7]1)[O:8][CH2:9][CH:10]([CH2:11][O:12][Si:13]([CH3:14])([CH3:15])[C:16]([CH3:17])([CH3:18])[CH3:19])[O:20]2
CC(C)(C)[Si](C)(C)OCC1COc2cc(Br)cnc2O1.CI
Cc1cnc2c(c1)OCC(CO[Si](C)(C)C(C)(C)C)O2
null
null
C1CCOC1
C-C Coupling
OtherReaction
7d02a1397677532c497b06779094a84b5891e297cb244a69d6935fe65c441acf
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1cnc2c(c1)OCCO2
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4](:[c:5](:[c:6]:1)-[#8:7])-[#8:8].I-[CH3;D1;+0:9]>>[#8:8]-[c:4]1:[#7;a:3]:[c:2]:[c;H0;D3;+0:1](-[CH3;D1;+0:9]):[c:6]:[c:5]:1-[#8:7]
41.9
[{"value": 41.9, "product": "CC(C)(C)[Si](OCC1COC=2C(=NC=C(C2)C)O1)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
75
MINUTE
Reaction under nitrogen atmosphere. A solution of intermediate (37) (0.00194 mol) in THF was cooled to −78° C. BuLi (0.00214 mol, 2.5M) was added dropwise and the mixture was stirred for 75 minutes at −78° C. Then, iodomethane (00214 mol) was added and the reaction mixture was stirred for 45 minutes. A saturated aqueou...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1cnc2c(c1)OCCO2
c1cnc2c(c1)OCCO2
c1cnc2c(c1)OCCO2
Br-.I-
C1CCOC1
-78
1.25
CC(C)(C)[Si](C)(C)OCC1COc2cc(Br)cnc2O1.CI>C1CCOC1>Cc1cnc2c(c1)OCC(CO[Si](C)(C)C(C)(C)C)O2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ae7b455778fa4904bb54a3c6f5dbc473
CS(=O)(=O)Cl.Cc1cnc2c(c1)OCC(CO)O2>>Cc1cnc2c(c1)OCC(COS(C)(=O)=O)O2
O.CS(=O)(=O)Cl.CC=1C=C2C(=NC1)OC(CO2)CO.C(C)N(CC)CC>>CS(=O)(=O)OCC1COC=2C(=NC=C(C2)C)O1
Cl[S:13]([CH3:14])(=[O:15])=[O:16].[CH3:1][c:2]1[cH:3][n:4][c:5]2[c:6]([cH:7]1)[O:8][CH2:9][CH:10]([CH2:11][OH:12])[O:17]2>>[CH3:1][c:2]1[cH:3][n:4][c:5]2[c:6]([cH:7]1)[O:8][CH2:9][CH:10]([CH2:11][O:12][S:13]([CH3:14])(=[O:15])=[O:16])[O:17]2
CS(=O)(=O)Cl.Cc1cnc2c(c1)OCC(CO)O2
Cc1cnc2c(c1)OCC(COS(C)(=O)=O)O2
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1cnc2c(c1)OCCO2
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#8:5]-[C:6]-[C:7]-[OH;D1;+0:8]>>[#8:5]-[C:6]-[C:7]-[O;H0;D2;+0:8]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
99
[{"value": 99.0, "product": "CS(=O)(=O)OCC1COC=2C(=NC=C(C2)C)O1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
Methanesulfonyl chloride (0.00103 mol) was added to a mixture of intermediate (39) (0.00081 mol) and triethylamine (0.0019 mol) in DCM, stirred at 0° C. The reaction mixture was stirred for 30 minutes at 0° C. Water was added. The organic layer was separated, dried, filtered and the solvent was evaporated, yielding 0.2...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1cnc2c(c1)OCCO2
HCl
C(Cl)Cl
0
null
CS(=O)(=O)Cl.Cc1cnc2c(c1)OCC(CO)O2>C(Cl)Cl>Cc1cnc2c(c1)OCC(COS(C)(=O)=O)O2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c3d23e65adee4b12b12b3b4c3cb07888
BrBr.O=S([O-])[O-].OC[C@H]1COc2cccnc2O1>>OCC1COc2c(Br)ccnc2O1.OC[C@H]1COc2cc(Br)cnc2O1
[O-]S(=O)[O-].[Na+].[Na+].O1C[C@@H](OC2=NC=CC=C21)CO.BrBr>>BrC=1C=C2C(=NC1)O[C@H](CO2)CO.BrC1=C2C(=NC=C1)OC(CO2)CO
[Br:8][Br:22].S([O-:13])(=[O:14])[O-:18].[OH:1][CH2:2][C@H:16]1[CH2:4][O:5][c:6]2[cH:7][cH:9][cH:10][n:11][c:12]2[O:26]1>>[OH:1][CH2:2][CH:3]1[CH2:4][O:5][c:6]2[c:7]([Br:8])[cH:9][cH:10][n:11][c:12]2[O:13]1.[OH:14][CH2:15][C@H:16]1[CH2:17][O:18][c:19]2[cH:20][c:21]([Br:22])[cH:23][n:24][c:25]2[O:26]1
BrBr.O=S([O-])[O-].OC[C@H]1COc2cccnc2O1
OCC1COc2c(Br)ccnc2O1.OC[C@H]1COc2cc(Br)cnc2O1
null
null
C(=O)([O-])[O-].[Na+].[Na+].C(Cl)Cl
Aromatic Heterocycle Formation
OtherReaction
06ddb3b84b1199052de7ea93a55acafccf7f1846e13a606e13fa1ca33162d4d4
767e0fc4b9104315cd7ac1893fa5e383fffd5da088a777a015169e9731cb9302
c1cnc2c(c1)OCCO2.c1cnc2c(c1)OCCO2
[Br;H0;D1;+0:1]-[Br;H0;D1;+0:2].[O-;H0;D1:3]-S(-[O-;H0;D1:4])=[O;H0;D1;+0:5].[O;D1;H1:6]-[CH2;D2;+0:7]-[C@H;D3;+0:8]1-[CH2;D2;+0:9]-[#8:10]-[c:11]2:[cH;D2;+0:12]:[c:13]:[c:14]:[#7;a:15]:[c;H0;D3;+0:16]:2-[O;H0;D2;+0:17]-1>>[Br;H0;D1;+0:2]-[c;H0;D3;+0:12]1:[c:13]:[c:14]:[#7;a:15]:[c;H0;D3;+0:16]2:[c:11]:1-[#8:10]-[CH2;D...
null
[]
null
null
16
HOUR
To a solution of intermediate (2-a) (0.03 mol) in DCM (50 ml) and Na2CO3 saturated (50 ml), bromine (0.09 mol) was added dropwise and the reaction mixture was stirred for 16 hours at room temperature. Then a Na2SO3-solution (10%) was added and the mixture was stirred for 5 minutes at room temperature and then neutraliz...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol
Aromatic halide.Aromatic halide.Ether.Ether.Ether.Ether.Primary alcohol.Primary alcohol
c1cnc2c(c1)OCCO2
c1cnc2c(c1)OCCO2.c1cnc2c(c1)OCCO2
c1cnc2c(c1)OCCO2.c1cnc2c(c1)OCCO2
null
C(=O)([O-])[O-].[Na+].[Na+].C(Cl)Cl
null
16
BrBr.O=S([O-])[O-].OC[C@H]1COc2cccnc2O1>C(=O)([O-])[O-].[Na+].[Na+].C(Cl)Cl>OCC1COc2c(Br)ccnc2O1.OC[C@H]1COc2cc(Br)cnc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7a5b96a352424d638904a6a376f3d613
CS(=O)(=O)Cl.OCC1COc2c(Br)ccnc2O1>>CS(=O)(=O)OC[C@@H]1COc2c(Br)ccnc2O1
BrC1=C2C(=NC=C1)OC(CO2)CO.C(C)N(CC)CC.CS(=O)(=O)Cl>>CS(=O)(=O)OC[C@@H]1COC=2C(=NC=CC2Br)O1
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][CH:7]1[CH2:8][O:9][c:10]2[c:11]([Br:12])[cH:13][cH:14][n:15][c:16]2[O:17]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][C@@H:7]1[CH2:8][O:9][c:10]2[c:11]([Br:12])[cH:13][cH:14][n:15][c:16]2[O:17]1
CS(=O)(=O)Cl.OCC1COc2c(Br)ccnc2O1
CS(=O)(=O)OC[C@@H]1COc2c(Br)ccnc2O1
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1cnc2c(c1)OCCO2
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#8:5]-[C:6]-[C:7]-[OH;D1;+0:8]>>[#8:5]-[C:6]-[C:7]-[O;H0;D2;+0:8]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
92.6
[{"value": 92.6, "product": "CS(=O)(=O)OC[C@@H]1COC=2C(=NC=CC2Br)O1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a mixture of intermediate (42) (0.0014 mol) and triethylamine (0.0028 mol) in DCM (5 ml), methanesulfonyl chloride (0.0021 mol) was slowly added at room temperature. The reaction mixture was stirred for 16 hours and was then extracted with water. The separated organic layer was dried, filtered and the solvent was ev...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1cnc2c(c1)OCCO2
HCl
C(Cl)Cl
null
16
CS(=O)(=O)Cl.OCC1COc2c(Br)ccnc2O1>C(Cl)Cl>CS(=O)(=O)OC[C@@H]1COc2c(Br)ccnc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1cb28e245e6246579ac3aca6c012a0d0
C=CCO.Oc1cnccc1Cl>>C=CCOc1cnccc1Cl
ClC1=C(C=NC=C1)O.C(C=C)O.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>ClC1=C(C=NC=C1)OCC=C
O[CH2:3][CH:2]=[CH2:1].[OH:4][c:5]1[cH:6][n:7][cH:8][cH:9][c:10]1[Cl:11]>>[CH2:1]=[CH:2][CH2:3][O:4][c:5]1[cH:6][n:7][cH:8][cH:9][c:10]1[Cl:11]
C=CCO.Oc1cnccc1Cl
C=CCOc1cnccc1Cl
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether
86bfb73617450d22f9456ed5ce4d96a73f1f8fc0c016bebae57fda68e2da86a2
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccncc1
O-[CH2;D2;+0:1]-[C:2]=[C;D1;H2:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]:[#7;a:8]:[c:9]>>[C;D1;H2:3]=[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]:[#7;a:8]:[c:9]
32.6
[{"value": 32.6, "product": "ClC1=C(C=NC=C1)OCC=C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of diazenedicarboxylic acid diethyl ester (0.1572 mol) in THF (163 ml) was added dropwise to a mixture of 4-chloro-3-pyridinol (0.1429 mol), 2-propen-1-ol (0.1572 mol) and triphenyl-phosphine (0.1572 mol) in THF (276 ml), that was cooled with an ice-water bath and under nitrogen flow. The formed mixture was ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
null
c1ccncc1
HO-
C1CCOC1
null
null
C=CCO.Oc1cnccc1Cl>C1CCOC1>C=CCOc1cnccc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-94d8148633e341e8970b0d1286e9d02e
BrCC(Br)COc1cnccc1OCc1ccccc1>>BrCC1COc2cnccc2O1
[NH4+].[Cl-].C(=O)([O-])C(O)C(O)C(=O)[O-].[Na+].[K+].BrC(COC=1C=NC=CC1OCC1=CC=CC=C1)CBr>>BrCC1OC2=C(C=NC=C2)OC1
Br[CH:3]([CH2:2][Br:1])[CH2:4][O:5][c:6]1[cH:7][n:8][cH:9][cH:10][c:11]1[O:12]Cc1ccccc1>>[Br:1][CH2:2][CH:3]1[CH2:4][O:5][c:6]2[cH:7][n:8][cH:9][cH:10][c:11]2[O:12]1
BrCC(Br)COc1cnccc1OCc1ccccc1
BrCC1COc2cnccc2O1
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
6a91d731e35d1f75b5cb1ee9b07680dfdeabd193bab631f6f8f7634763bc665e
90564897fbe442dd5134de6abc48403858bfdbcd71e4ddc209af85b5258412e4
c1cc2c(cn1)OCCO2
Br-[CH;D3;+0:1](-[C:2]-[Br;D1;H0:3])-[C:4]-[#8:5]-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[c:10]:[c:11]:1-[O;H0;D2;+0:12]-C-c1:c:c:c:c:c:1>>[Br;D1;H0:3]-[C:2]-[CH;D3;+0:1]1-[C:4]-[#8:5]-[c:6]2:[c:7]:[#7;a:8]:[c:9]:[c:10]:[c:11]:2-[O;H0;D2;+0:12]-1
13.6
[{"value": 13.6, "product": "BrCC1OC2=C(C=NC=C2)OC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of intermediate (46) (0.0166 mol) in DCM (270 ml), FeCl3 (0.033 mol) was added portionwise and the mixture was stirred at room temperature overnight. The reaction mixture was treated with a saturated NH4Cl-solution and with a diluted solution of potassium sodium tartrate and then it was filtered off over ...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Ether
Ether
c1ccccc1
c1cc2c(cn1)OCCO2
c1cc2c(cn1)OCCO2
HBr
C(Cl)Cl
null
8
BrCC(Br)COc1cnccc1OCc1ccccc1>C(Cl)Cl>BrCC1COc2cnccc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-163dcc41d9d344648276574598d51bb8
Brc1cncnc1.C=CCO>>C=CCOc1cncnc1
BrC=1C=NC=NC1.C(C=C)O.[H-].[Na+]>>C(C=C)OC=1C=NC=NC1
Br[c:5]1[cH:6][n:7][cH:8][n:9][cH:10]1.[CH2:1]=[CH:2][CH2:3][OH:4]>>[CH2:1]=[CH:2][CH2:3][O:4][c:5]1[cH:6][n:7][cH:8][n:9][cH:10]1
Brc1cncnc1.C=CCO
C=CCOc1cncnc1
null
null
O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
a445000eb5ed501274d93689ad5b9d45095af02deca02b6b541c8a834890a276
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1cncnc1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1.[C;D1;H2:7]=[C:8]-[C:9]-[OH;D1;+0:10]>>[C;D1;H2:7]=[C:8]-[C:9]-[O;H0;D2;+0:10]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1
26.8
[{"value": 26.8, "product": "C(C=C)OC=1C=NC=NC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
5-Bromo-pyrimidine (0.063 mol) was slowly added to 2-propen-1-ol (4.03 mol) at 0° C. and this mixture was stirred at room temperature for 1 hour. Then NaH 60% (0.126 mol) was added and the reaction mixture was stirred and refluxed for 48 hours. Water was added and the mixture was extracted with ethyl acetate. The separ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cncnc1
c1cncnc1
c1cncnc1
HBr
O
null
1
Brc1cncnc1.C=CCO>O>C=CCOc1cncnc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-40f74aa4c754468cb801ca900ccfeaa9
O=c1[nH]cncc1OCC(Br)CBr>>BrCC1COc2cncnc2O1
BrC(COC=1C(NC=NC1)=O)CBr.C(=O)(O)[O-].[Na+]>>BrCC1COC2=C(N=CN=C2)O1
Br[CH:3]([CH2:2][Br:1])[CH2:4][O:5][c:6]1[cH:7][n:8][cH:9][nH:10][c:11]1=[O:12]>>[Br:1][CH2:2][CH:3]1[CH2:4][O:5][c:6]2[cH:7][n:8][cH:9][n:10][c:11]2[O:12]1
O=c1[nH]cncc1OCC(Br)CBr
BrCC1COc2cncnc2O1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
2cf40f24d2b2806e3617773e4e35db40e12cd8a43ab5a32e7bc2002e284bce4a
302f6042868059cd60da1fdb36403ed695deb6b9677d3cdc596dc8b229cbf806
c1ncc2c(n1)OCCO2
Br-[CH;D3;+0:1](-[C:2]-[Br;D1;H0:3])-[C:4]-[#8:5]-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[nH;D2;+0:10]:[c;H0;D3;+0:11]:1=[O;H0;D1;+0:12]>>[Br;D1;H0:3]-[C:2]-[CH;D3;+0:1]1-[C:4]-[#8:5]-[c:6]2:[c:7]:[#7;a:8]:[c:9]:[n;H0;D2;+0:10]:[c;H0;D3;+0:11]:2-[O;H0;D2;+0:12]-1
52.3
[{"value": 52.3, "product": "BrCC1COC2=C(N=CN=C2)O1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of intermediate (50) (0.0091 mol) and NaHCO3 (0.0113 mol) in ethanol (100 ml) was stirred and refluxed for 16 hours. The reaction mixture was allowed to cool to room temperature and the solvent was evaporated. The residue was taken up in water and ethyl acetate. The separated organic layer was dried, filtered...
10.6084/m9.figshare.5104873.v1
null
Secondary halide
Ether
c1cncnc1
c1ncc2c(n1)OCCO2
c1ncc2c(n1)OCCO2
HBr
C(C)O
null
null
O=c1[nH]cncc1OCC(Br)CBr>C(C)O>BrCC1COc2cncnc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b5cf7d59486349e89fab2b0620de818e
C=CC(=O)OCC.NCCCN(Cc1ccccc1)Cc1ccccc1>>CCOC(=O)CCNCCCN(Cc1ccccc1)Cc1ccccc1
NCCCN(CC1=CC=CC=C1)CC1=CC=CC=C1.C(C=C)(=O)OCC>>C1(=CC=CC=C1)CN(CCCNCCC(=O)OCC)CC1=CC=CC=C1
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]=[CH2:7].[NH2:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1)[CH2:20][c:21]1[cH:22][cH:23][cH:24][cH:25][cH:26]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH2:7][NH:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19...
C=CC(=O)OCC.NCCCN(Cc1ccccc1)Cc1ccccc1
CCOC(=O)CCNCCCN(Cc1ccccc1)Cc1ccccc1
null
null
C(C)O
Heteroatom Alkylation and Arylation
aza-Michael addition primary
1a11d98577799a07170cd5efd9dd7bb03f34d533a77a248c8322bf305dad4248
d462df48e06a3b2a50bc83cb7c56b836b8a054b4c300671faa54924b570d58bc
c1ccc(CNCc2ccccc2)cc1
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH;D2;+0:5]=[CH2;D1;+0:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[CH2;D2;+0:6]-[CH2;D2;+0:5]-[C:3](=[O;D1;H0:4])-[#8:2]-[C:1]
39.1
[{"value": 39.1, "product": "C1(=CC=CC=C1)CN(CCCNCCC(=O)OCC)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Reaction under an argon flow. A mixture of 1-amino-3-dibenzylaminopropane (0.195 mol) in ethanol (225 ml) was stirred at room temperature. Ethyl propenoate (0.2 mol) was poured into the mixture and the reaction mixture was stirred overnight at room temperature. The solvent was evaporated. The residue was purified by co...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine.Vinyl
Ester.Secondary amine
null
null
c1ccccc1.c1ccccc1
null
C(C)O
null
null
C=CC(=O)OCC.NCCCN(Cc1ccccc1)Cc1ccccc1>C(C)O>CCOC(=O)CCNCCCN(Cc1ccccc1)Cc1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-00e861ed9a3041e892dd9e16a65da7fc
CCOC(=O)CCNCCCN(Cc1ccccc1)Cc1ccccc1>>O=C1CCN(CCCN(Cc2ccccc2)Cc2ccccc2)C(=O)N1
Cl.O([K])C#N.O([K])C#N.Cl.CC(C)O.C1(=CC=CC=C1)CN(CCCNCCC(=O)OCC)CC1=CC=CC=C1>>C1(=CC=CC=C1)CN(CCCN1C(NC(CC1)=O)=O)CC1=CC=CC=C1
CCO[C:2](=[O:1])[CH2:3][CH2:4][NH:5][CH2:6][CH2:7][CH2:8][N:9]([CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1>>[O:1]=[C:2]1[CH2:3][CH2:4][N:5]([CH2:6][CH2:7][CH2:8][N:9]([CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[CH2:17][c:18]2[cH:19][cH:20][cH:21][cH:2...
CCOC(=O)CCNCCCN(Cc1ccccc1)Cc1ccccc1
O=C1CCN(CCCN(Cc2ccccc2)Cc2ccccc2)C(=O)N1
null
O([K])C#N
O.CO.C(C)O
Miscellaneous
OtherReaction
5313f292ded8b0c9c26323ff4af309b7e6ca577a3652c823683591f43f7bff01
431191b6e72cab06c234e878107510e04274523c51fab9db3aa00f4c030b4555
O=C1CCN(CCCN(Cc2ccccc2)Cc2ccccc2)C(=O)N1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]-[NH;D2;+0:5]-[C:6]-[C:7]>>[C:7]-[C:6]-[N;H0;D3;+0:5]1-[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:8]-[C:9]-1=[O;D1;H0:10]
null
[]
null
null
15
MINUTE
Intermediate (52) was stirred in ethanol (150 ml). The mixture was acidified with HCl/2-propanol (±60 ml)+water (2 ml). The mixture was stirred for 15 minutes. The solvent was evaporated at 60° C. Ethanol was added to the residue. The solvent was evaporated. A mixture of methanol in water (70:30; 200 ml) was added to t...
10.6084/m9.figshare.5104873.v1
null
Ester.Secondary amine
Urea.Unsubstituted dicarboximide
null
C1CNC[NH]C1
C1CNC[NH]C1.c1ccccc1.c1ccccc1
null
O([K])C#N.O.CO.C(C)O
null
0.25
CCOC(=O)CCNCCCN(Cc1ccccc1)Cc1ccccc1>O([K])C#N.O.CO.C(C)O>O=C1CCN(CCCN(Cc2ccccc2)Cc2ccccc2)C(=O)N1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c93706c944af46a08c77f879d28febb2
O=C1CCN(CCCN(Cc2ccccc2)Cc2ccccc2)C(=O)N1>>NCCCN1CCC(=O)NC1=O
C1(=CC=CC=C1)CN(CCCN1C(NC(CC1)=O)=O)CC1=CC=CC=C1.[H][H]>>NCCCN1C(NC(CC1)=O)=O
c1ccc(C[N:1](Cc2ccccc2)[CH2:2][CH2:3][CH2:4][N:5]2[CH2:6][CH2:7][C:8](=[O:9])[NH:10][C:11]2=[O:12])cc1>>[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][C:8](=[O:9])[NH:10][C:11]1=[O:12]
O=C1CCN(CCCN(Cc2ccccc2)Cc2ccccc2)C(=O)N1
NCCCN1CCC(=O)NC1=O
null
[Pd]
CO
Deprotection
OtherReaction
2d0141567e42eb1f1e525678ba93b1f94e67edd4ce8af946d59aa7922040fcc6
09463156f8971f4e8007d84d8ed410eed1d618bdb6ba7dd05b4970ff2019f62b
O=C1CCNC(=O)N1
[C:1]-[C:2]-[N;H0;D3;+0:3](-C-c1:c:c:c:c:c:1)-C-c1:c:c:c:c:c:1>>[C:1]-[C:2]-[NH2;D1;+0:3]
90
[{"value": 90.0, "product": "NCCCN1C(NC(CC1)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of intermediate (53) (0.010 mol) in methanol (150 ml) was hydrogenated at 50° C. with palladium-on-carbon (10%, 1 g) as a catalyst. After uptake of hydrogen (2 equivalents), the catalyst was filtered off and the filtrate was evaporated. Toluene was added and azeotroped on the rotary evaporator. The residue wa...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Primary amine
c1ccccc1.c1ccccc1
null
C1C[NH]CNC1
Other
[Pd].CO
null
null
O=C1CCN(CCCN(Cc2ccccc2)Cc2ccccc2)C(=O)N1>[Pd].CO>NCCCN1CCC(=O)NC1=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b9164710d6a9432fba83d9bfa12c024f
CC1(C)CNC(=O)N(CCCN)C1.CS(=O)(=O)OCC1Oc2cccnc2O1>>CC1(C)CNC(=O)N(CCCNCC2Oc3cccnc3O2)C1
CS(=O)(=O)OCC1OC=2C(=NC=CC2)O1.NCCCN1C(NCC(C1)(C)C)=O>>O1C(OC2=NC=CC=C21)CNCCCN2C(NCC(C2)(C)C)=O
[CH3:1][C:2]1([CH3:3])[CH2:4][NH:5][C:6](=[O:7])[N:8]([CH2:9][CH2:10][CH2:11][NH2:12])[CH2:23]1.CS(=O)(=O)O[CH2:13][CH:14]1[O:15][c:16]2[cH:17][cH:18][cH:19][n:20][c:21]2[O:22]1>>[CH3:1][C:2]1([CH3:3])[CH2:4][NH:5][C:6](=[O:7])[N:8]([CH2:9][CH2:10][CH2:11][NH:12][CH2:13][CH:14]2[O:15][c:16]3[cH:17][cH:18][cH:19][n:20][...
CC1(C)CNC(=O)N(CCCN)C1.CS(=O)(=O)OCC1Oc2cccnc2O1
CC1(C)CNC(=O)N(CCCNCC2Oc3cccnc3O2)C1
null
null
null
Heteroatom Alkylation and Arylation
Alkylation of amines
8445343b2fb2fd8a9bc06f8532794f2ba6b99565a6e05a3bb9a4344ce2671186
7e6303acde8be57b43b4c6a673e1c7537b1efde90f08932e09e153dbba53a700
O=C1NCCCN1CCCNCC1Oc2cccnc2O1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]1-[#8:3]-[c:4]:[c:5](:[#7;a:6])-[#8:7]-1.[C:8]-[C:9]-[NH2;D1;+0:10]>>[#7;a:6]:[c:5]1:[c:4]-[#8:3]-[C:2](-[CH2;D2;+0:1]-[NH;D2;+0:10]-[C:9]-[C:8])-[#8:7]-1
50.2
[{"value": 50.2, "product": "O1C(OC2=NC=CC=C21)CNCCCN2C(NCC(C2)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
2
HOUR
A mixture of intermediate (6) (0.0092 mol) and intermediate (13) (0.0183 mol) was stirred for 2 hours at 100° C. The crude reaction mixture was purified by open column chromatography over silica gel (eluent: CH2Cl2/CH3OH 90/10). The desired fractions were collected and the solvent was evaporated. The residue was washed...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Primary amine
Secondary amine
null
null
C1CNC[NH]C1.c1cnc2c(c1)OCO2
MsOH.HO-
null
100
2
CC1(C)CNC(=O)N(CCCN)C1.CS(=O)(=O)OCC1Oc2cccnc2O1>>CC1(C)CNC(=O)N(CCCNCC2Oc3cccnc3O2)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-272890ddb56549ff8e10cff7c32a370c
O=C1CN(CC2CO2)C(=O)N1.c1ccc(CNCC2COc3cccnc3O2)cc1>>O=C1CN(CC(O)CN(Cc2ccccc2)CC2COc3cccnc3O2)C(=O)N1
C1(=CC=CC=C1)CNCC1COC=2C(=NC=CC2)O1.O1C(C1)CN1C(NC(C1)=O)=O>>O1CC(OC2=NC=CC=C21)CN(CC(CN2C(NC(C2)=O)=O)O)CC2=CC=CC=C2
[O:1]=[C:2]1[CH2:3][N:4]([CH2:5][CH:6]2[O:7][CH2:8]2)[C:28](=[O:29])[NH:30]1.[NH:9]([CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[CH2:17][CH:18]1[CH2:19][O:20][c:21]2[cH:22][cH:23][cH:24][n:25][c:26]2[O:27]1>>[O:1]=[C:2]1[CH2:3][N:4]([CH2:5][CH:6]([OH:7])[CH2:8][N:9]([CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c...
O=C1CN(CC2CO2)C(=O)N1.c1ccc(CNCC2COc3cccnc3O2)cc1
O=C1CN(CC(O)CN(Cc2ccccc2)CC2COc3cccnc3O2)C(=O)N1
null
null
CO
Heteroatom Alkylation and Arylation
Ring opening of epoxide with amine
8b0e6adfb78f36f9ea38287644fe13d1ed2aa3ea65e10cc66a65b05c37e2e473
97e758d6c4c8255d25541eb6c6a6f62e7dc30829ea162ca3392731efabc98a65
O=C1CN(CCCN(Cc2ccccc2)CC2COc3cccnc3O2)C(=O)N1
[#8:1]-[C:2]-[C:3]-[NH;D2;+0:4]-[C:5]-[c:6].[C:7]-[C:8]1-[CH2;D2;+0:9]-[O;H0;D2;+0:10]-1>>[#8:1]-[C:2]-[C:3]-[N;H0;D3;+0:4](-[C:5]-[c:6])-[CH2;D2;+0:9]-[C:8](-[C:7])-[OH;D1;+0:10]
62.9
[{"value": 62.9, "product": "O1CC(OC2=NC=CC=C21)CN(CC(CN2C(NC(C2)=O)=O)O)CC2=CC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 2,3-dihydro-N-(phenylmethyl)-1,4dioxino[2,3-b]pyridine-3-methanamine (0.0059 mol) and intermediate (18) (0.00497 mol) in methanol (30 ml) was stirred and refluxed overnight. The solvent was evaporated. The residue was purified by short open column chromatography over silica gel (eluent: CH2Cl212-propanone ...
10.6084/m9.figshare.5104873.v1
null
Ether.Secondary amine
Secondary alcohol.Tertiary amine
C1CO1
null
C1C[NH]CN1.c1ccccc1.c1cnc2c(c1)OCCO2
null
CO
null
null
O=C1CN(CC2CO2)C(=O)N1.c1ccc(CNCC2COc3cccnc3O2)cc1>CO>O=C1CN(CC(O)CN(Cc2ccccc2)CC2COc3cccnc3O2)C(=O)N1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c60ac8e4ac2c4b1f93c294d3f5c814f1
CS(=O)(=O)OC[C@@H]1COc2cccnc2O1.NCCCN1CCC(=O)NC1=O>>O=C1CCN(CCCNC[C@H]2COc3cccnc3O2)C(=O)N1
NCCCN1C(NC(CC1)=O)=O.CS(=O)(=O)OC[C@@H]1COC=2C(=NC=CC2)O1>>O1C[C@@H](OC2=NC=CC=C21)CNCCCN2C(NC(CC2)=O)=O
CS(=O)(=O)O[CH2:10][C@@H:11]1[CH2:12][O:13][c:14]2[cH:15][cH:16][cH:17][n:18][c:19]2[O:20]1.[O:1]=[C:2]1[CH2:3][CH2:4][N:5]([CH2:6][CH2:7][CH2:8][NH2:9])[C:21](=[O:22])[NH:23]1>>[O:1]=[C:2]1[CH2:3][CH2:4][N:5]([CH2:6][CH2:7][CH2:8][NH:9][CH2:10][C@H:11]2[CH2:12][O:13][c:14]3[cH:15][cH:16][cH:17][n:18][c:19]3[O:20]2)[C:...
CS(=O)(=O)OC[C@@H]1COc2cccnc2O1.NCCCN1CCC(=O)NC1=O
O=C1CCN(CCCNC[C@H]2COc3cccnc3O2)C(=O)N1
null
null
O1CCOCC1
Heteroatom Alkylation and Arylation
Alkylation of amines
8445343b2fb2fd8a9bc06f8532794f2ba6b99565a6e05a3bb9a4344ce2671186
7e6303acde8be57b43b4c6a673e1c7537b1efde90f08932e09e153dbba53a700
O=C1CCN(CCCNC[C@H]2COc3cccnc3O2)C(=O)N1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2](-[#8:3]-[c:4]:[#7;a:5])-[C:6]-[#8:7].[C:8]-[C:9]-[NH2;D1;+0:10]>>[#7;a:5]:[c:4]-[#8:3]-[C:2](-[CH2;D2;+0:1]-[NH;D2;+0:10]-[C:9]-[C:8])-[C:6]-[#8:7]
16.1
[{"value": 16.1, "product": "O1C[C@@H](OC2=NC=CC=C21)CNCCCN2C(NC(CC2)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of intermediate (54) (0.058 mol) in dioxane (400 ml) was stirred. A mixture of intermediate (3) (0.029 mol) and CaO (2.4 g) was added. The reaction mixture was stirred at 140° C. for 16 hours. The solvent was evaporated. DCM and water was added to the residue. The separated organic layer was dried, filtered a...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Primary amine
Secondary amine
null
null
C1CNC[NH]C1.c1cnc2c(c1)OCCO2
MsOH.HO-
O1CCOCC1
null
null
CS(=O)(=O)OC[C@@H]1COc2cccnc2O1.NCCCN1CCC(=O)NC1=O>O1CCOCC1>O=C1CCN(CCCNC[C@H]2COc3cccnc3O2)C(=O)N1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5e097a300e7d4722996dea0fb55be713
CS(=O)(=O)OC[C@@H]1COc2cccnc2O1.NCc1ccccc1>>c1ccc(CNC[C@H]2COc3cccnc3O2)cc1
CS(=O)(=O)OC[C@@H]1COC=2C(=NC=CC2)O1.C(C1=CC=CC=C1)N.C(=O)(O)[O-].[Na+]>>C1(=CC=CC=C1)CNC[C@H]1COC=2C(=NC=CC2)O1
CS(=O)(=O)O[CH2:7][C@@H:8]1[CH2:9][O:10][c:11]2[cH:12][cH:13][cH:14][n:15][c:16]2[O:17]1.[cH:1]1[cH:2][cH:3][c:4]([CH2:5][NH2:6])[cH:18][cH:19]1>>[cH:1]1[cH:2][cH:3][c:4]([CH2:5][NH:6][CH2:7][C@H:8]2[CH2:9][O:10][c:11]3[cH:12][cH:13][cH:14][n:15][c:16]3[O:17]2)[cH:18][cH:19]1
CS(=O)(=O)OC[C@@H]1COc2cccnc2O1.NCc1ccccc1
c1ccc(CNC[C@H]2COc3cccnc3O2)cc1
null
null
O1CCOCC1
Heteroatom Alkylation and Arylation
Alkylation of amines
8445343b2fb2fd8a9bc06f8532794f2ba6b99565a6e05a3bb9a4344ce2671186
7e6303acde8be57b43b4c6a673e1c7537b1efde90f08932e09e153dbba53a700
c1ccc(CNC[C@H]2COc3cccnc3O2)cc1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2](-[#8:3]-[c:4]:[#7;a:5])-[C:6]-[#8:7].[NH2;D1;+0:8]-[C:9]-[c:10]>>[#7;a:5]:[c:4]-[#8:3]-[C:2](-[CH2;D2;+0:1]-[NH;D2;+0:8]-[C:9]-[c:10])-[C:6]-[#8:7]
null
[]
null
null
null
null
A mixture of intermediate (3) (0.041 mol), benzylamine (0.041 mol) and NaHCO3 (0.11 mol) in dioxane (100 ml) was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was taken up in water and DCM. The separated organic layer was dried, filtered and the solvent was evaporated. The residue was purif...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Primary amine
Secondary amine
null
null
c1ccccc1.c1cnc2c(c1)OCCO2
MsOH.HO-
O1CCOCC1
null
null
CS(=O)(=O)OC[C@@H]1COc2cccnc2O1.NCc1ccccc1>O1CCOCC1>c1ccc(CNC[C@H]2COc3cccnc3O2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-38297af7c6ec49538e0643e0ab7da876
C=CC#N.c1ccc(CNC[C@H]2COc3cccnc3O2)cc1>>N#CCCN(Cc1ccccc1)C[C@H]1COc2cccnc2O1
C(C=C)#N.C1(=CC=CC=C1)CNC[C@H]1COC=2C(=NC=CC2)O1.C(C=C)#N.C(C=C)#N.C(C=C)#N>>O1C[C@@H](OC2=NC=CC=C21)CN(CCC#N)CC2=CC=CC=C2
[N:1]#[C:2][CH:3]=[CH2:4].[NH:5]([CH2:6][c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1)[CH2:13][C@H:14]1[CH2:15][O:16][c:17]2[cH:18][cH:19][cH:20][n:21][c:22]2[O:23]1>>[N:1]#[C:2][CH2:3][CH2:4][N:5]([CH2:6][c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1)[CH2:13][C@H:14]1[CH2:15][O:16][c:17]2[cH:18][cH:19][cH:20][n:21][c:22]2[O:23]1
C=CC#N.c1ccc(CNC[C@H]2COc3cccnc3O2)cc1
N#CCCN(Cc1ccccc1)C[C@H]1COc2cccnc2O1
null
null
C(C)O
Heteroatom Alkylation and Arylation
aza-Michael addition secondary
8acf647a588bdc7347506dcd3290904024f41acb450fe55eb6c0af193ad82ab8
828fcbb87adfef9f22c9a1e52b43c3df76cb2e49bfe62b57e8b79965772a2bed
c1ccc(CNC[C@H]2COc3cccnc3O2)cc1
[#8:1]-[C:2]-[C:3]-[NH;D2;+0:4]-[C:5]-[c:6].[CH2;D1;+0:7]=[CH;D2;+0:8]-[C:9]#[N;D1;H0:10]>>[#8:1]-[C:2]-[C:3]-[N;H0;D3;+0:4](-[C:5]-[c:6])-[CH2;D2;+0:7]-[CH2;D2;+0:8]-[C:9]#[N;D1;H0:10]
99.5
[{"value": 99.5, "product": "O1C[C@@H](OC2=NC=CC=C21)CN(CCC#N)CC2=CC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Intermediate (55) (0.0195 mol) was dissolved in ethanol (50 ml). 2-Propenenitrile (0.02 mol) was added and the reaction mixture was stirred and refluxed overnight. Additional 2-propenenitrile (0.02 mol) was added and the reaction mixture was stirred and refluxed for 2 hours. Additional 2-propenenitrile (0.02 mol) was a...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Vinyl
Tertiary amine
null
null
c1ccccc1.c1cnc2c(c1)OCCO2
null
C(C)O
null
null
C=CC#N.c1ccc(CNC[C@H]2COc3cccnc3O2)cc1>C(C)O>N#CCCN(Cc1ccccc1)C[C@H]1COc2cccnc2O1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-75ed49acc2784c3493ed5ba4a7dabfe7
CCOCC.Nc1ccc(Br)cc1C(=O)O>>CC(C)(O)c1cc(Br)ccc1N
Cl.NC1=C(C(=O)O)C=C(C=C1)Br.C[Mg]Br.CCOCC.[OH-].[Na+]>>NC1=C(C=C(C=C1)Br)C(C)(C)O
CCOC[CH3:3].O=[C:2]([OH:4])[c:5]1[cH:6][c:7]([Br:8])[cH:9][cH:10][c:11]1[NH2:12]>>[CH3:1][C:2]([CH3:3])([OH:4])[c:5]1[cH:6][c:7]([Br:8])[cH:9][cH:10][c:11]1[NH2:12]
CCOCC.Nc1ccc(Br)cc1C(=O)O
CC(C)(O)c1cc(Br)ccc1N
null
null
C(C)(=O)OCC.C1CCOC1
C-C Coupling
OtherReaction
8fffede311ab6e976b2c87246cb985fbcf7b3efb2fae50d4a939c6943cabc726
4fb8cd12751de39cc525c444cef492bee5116e308d33a4cbda36c3aed28708a2
c1ccccc1
C-C-O-C-[CH3;D1;+0:1].O=[C;H0;D3;+0:2](-[O;D1;H1:3])-[c:4](:[c:5]):[c:6]>>[C;D1;H3:7]-[C;H0;D4;+0:2](-[CH3;D1;+0:1])(-[O;D1;H1:3])-[c:4](:[c:5]):[c:6]
57
[{"value": 57.0, "product": "NC1=C(C=C(C=C1)Br)C(C)(C)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
48
HOUR
A solution of 2-amino-5-bromobenzoic acid (10 g, 46 mmol) in dry THF (200 mL) was treated at −78° C. under nitrogen with a solution of methylmagnesium bromide in ether (3.0 M, 90 mL, 270 mmol). The reaction mixture was slowly warmed to ambient temperature, kept stirring for 48 hours under nitrogen and then poured into ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ether
Tertiary alcohol
null
null
c1ccccc1
HO-
C(C)(=O)OCC.C1CCOC1
null
48
CCOCC.Nc1ccc(Br)cc1C(=O)O>C(C)(=O)OCC.C1CCOC1>CC(C)(O)c1cc(Br)ccc1N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1bdb0c9c30984b148cab296c799186b4
CC(C)(O)c1cc(Br)ccc1N.O=C(n1ccnc1)n1ccnc1>>CC1(C)OC(=O)Nc2ccc(Br)cc21
NC1=C(C=C(C=C1)Br)C(C)(C)O.C(=O)(N1C=NC=C1)N1C=NC=C1>>BrC1=CC2=C(NC(OC2(C)C)=O)C=C1
[CH3:1][C:2]([CH3:3])([OH:4])[c:14]1[c:8]([NH2:7])[cH:9][cH:10][c:11]([Br:12])[cH:13]1.c1cn([C:5](n2ccnc2)=[O:6])cn1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11]([Br:12])[cH:13][c:14]21
CC(C)(O)c1cc(Br)ccc1N.O=C(n1ccnc1)n1ccnc1
CC1(C)OC(=O)Nc2ccc(Br)cc21
null
null
C1CCOC1
Protection
OtherReaction
862364157177f41c9bd3cedddf1e8ac68669ae6aef579bc9f5124c2f2002b152
37a2f72522e1c6135c1e724ca4e9730fb0d5786b25469510c29abe3444ce965b
O=C1Nc2ccccc2CO1
[C;D1;H3:1]-[C:2](-[C;D1;H3:3])(-[OH;D1;+0:4])-[c:5]:[c:6](-[NH2;D1;+0:7]):[c:8].[O;D1;H0:9]=[C;H0;D3;+0:10](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[C;D1;H3:1]-[C:2]1(-[C;D1;H3:3])-[O;H0;D2;+0:4]-[C;H0;D3;+0:10](=[O;D1;H0:9])-[NH;D2;+0:7]-[c:6](:[c:8]):[c:5]-1
100
[{"value": 100.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
50
CELSIUS
null
null
To a solution of 2-(2-amino-5-bromophenyl)propan-2-ol (18 g, 78 mmol) in dry THF (150 mL) was added 1,1′-carbonyldiimidazole (15.5 g, 94 mmol) under nitrogen. The reaction solution was heated at 50° C. overnight. The solvent was removed in vacuo and the residue was dissolved in ethyl acetate (100 mL). The solution was ...
10.6084/m9.figshare.5104873.v1
null
Tertiary alcohol.Primary amine
Carbamic ester
c1c[nH]cn1.c1c[nH]cn1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2
Other
C1CCOC1
50
null
CC(C)(O)c1cc(Br)ccc1N.O=C(n1ccnc1)n1ccnc1>C1CCOC1>CC1(C)OC(=O)Nc2ccc(Br)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dce1481c01604b6eb9f28444a07ed038
CC(C)OB(OC(C)C)OC(C)C.CC1(C)OC(=O)Nc2ccc(Br)cc21>>CC1(C)OC(=O)Nc2ccc(B(O)O)cc21
B(OC(C)C)(OC(C)C)OC(C)C.BrC1=CC2=C(NC(OC2(C)C)=O)C=C1.[Li]CCCC.CCCCCC>>CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C
CC(C)O[B:12]([O:13]C(C)C)[O:14]C(C)C.Br[c:11]1[cH:10][cH:9][c:8]2[c:16]([cH:15]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11]([B:12]([OH:13])[OH:14])[cH:15][c:16]21
CC(C)OB(OC(C)C)OC(C)C.CC1(C)OC(=O)Nc2ccc(Br)cc21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21
null
null
C1CCOC1
Miscellaneous
Preparation of boronic acids
2b0a2085eefa9fa3bf4ba7b9aabc03f175f26d8afa15449be7fcd2d2bb691b2a
dafd25fbe01879c365f8c874026e570f49824f4bb82016b29d0c5d21aeb58ca3
O=C1Nc2ccccc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].C-C(-C)-O-[B;H0;D3;+0:6](-[O;H0;D2;+0:7]-C(-C)-C)-[O;H0;D2;+0:8]-C(-C)-C>>[OH;D1;+0:7]-[B;H0;D3;+0:6](-[OH;D1;+0:8])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
81.2
[{"value": 81.0, "product": "CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 81.2, "product": "CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
30
MINUTE
To a solution of 6-bromo-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one (2 g, 7.8 mmol) in anhydrous THF (60 mL) was added a solution of n-BuLi in hexane (10 M, 2.4 mL, 24 mmol) at −78° C. under nitrogen. After stirring at −78° C. for 30 minutes, a slurry was obtained and treated with triisopropyl borate (6.5 mL, 2...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Boronic acid
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2
HBr
C1CCOC1
-78
0.5
CC(C)OB(OC(C)C)OC(C)C.CC1(C)OC(=O)Nc2ccc(Br)cc21>C1CCOC1>CC1(C)OC(=O)Nc2ccc(B(O)O)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c56b7eebb6a041479df5e59be7a069dc
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1cccc(Cl)c1>>CC1(C)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
BrC1=CC2=C(NC(OC2(C)C)=O)C=C1.ClC=1C=C(C=CC1)B(O)O.C([O-])([O-])=O.[Na+].[Na+]>>ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=O)C=C1
Br[c:11]1[cH:10][cH:9][c:8]2[c:20]([cH:19]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.OB(O)[c:12]1[cH:13][cH:14][cH:15][c:16]([Cl:17])[cH:18]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([Cl:17])[cH:18]3)[cH:19][c:20]21
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1cccc(Cl)c1
CC1(C)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
null
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1
O.COCCOC
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:8]:[c:7]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:9]:[c:10]
82.5
[{"value": 82.0, "product": "ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=O)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.5, "product": "ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=O)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
A mixture of 6-bromo-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one (1.5 g, 5.9 mmol), 3-chlorophenyl boronic acid (1.83 g, 11.7 mmol), tetrakis(triphenylphosphine)-palladium (0) (0.35 g, 0.3 mmol), and sodium carbonate (2.48 g, 23.4 mmol) in a mixture of DME and water (40 mL/10 mL) was degassed to remove the oxyge...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.O.COCCOC
85
null
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1cccc(Cl)c1>[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.O.COCCOC>CC1(C)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e4aeb5dbae2c48daa29afde8631fb69a
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(Br)cc(Br)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC1=CC(=CC(=C1)F)Br.C([O-])([O-])=O.[Na+].[Na+]>>BrC=1C=C(C=C(C1)F)C1=CC2=C(NC(OC2(C)C)=O)C=C1
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:21]([cH:20]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][c:14]([F:15])[cH:16][c:17]([Br:18])[cH:19]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([F:15])[cH:16][c:17]([Br:18])[cH:19]3)[cH:20][c:21]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(Br)cc(Br)c1
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21
null
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1
O.COCCOC
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
40
[{"value": 40.0, "product": "BrC=1C=C(C=C(C1)F)C1=CC2=C(NC(OC2(C)C)=O)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 40.0, "product": "BrC=1C=C(C=C(C1)F)C1=CC2=C(NC(OC2(C)C)=O)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
A mixture of (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid (2.22 g, 10 mmol), 1,3-dibromo-5-fluorobenzene (3.05 g, 12 mmol), tetrakis(triphenylphosphine)palladium (0) (0.6 g, 0.52 mmol), and sodium carbonate (2.2 g, 21 mmol) in a mixture of DME and water (70 mL/15 mL) was degassed to remove the ox...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.O.COCCOC
85
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(Br)cc(Br)c1>C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.O.COCCOC>CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c605e453a603463e80be6c8434fee87e
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21>>CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21
BrC=1C=C(C=C(C1)F)C1=CC2=C(NC(OC2(C)C)=O)C=C1.CN(C)C=O>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(C#N)C=C(C2)F)C
Br[c:17]1[cH:16][c:14]([F:15])[cH:13][c:12](-[c:11]2[cH:10][cH:9][c:8]3[c:22]([cH:21]2)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]3)[cH:20]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([F:15])[cH:16][c:17]([C:18]#[N:19])[cH:20]3)[cH:21][c:22]21
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21
null
[Zn].[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1
null
Miscellaneous
OtherReaction
3ae4da8b7f110de99cf8afc091b6f0c8540050148e425770f8030bce1480042c
73a96fe5e833259ca394a42f82d6cc2ee7231bcde92d95030d2893b90c3fef76
O=C1Nc2ccc(-c3ccccc3)cc2CO1
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]
84
[{"value": 84.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
A mixture of 6-(3-bromo-5-fluorophenyl)-4,4-dimethyl-2H-benz[d][1,3]oxazin-2-one (1 g, 2.8 mmol), zinc cyamide (0.2 g, 1.7 mmol), and tetrakis(triphenylphosphine)-palladium (0) (0.2 g, 0.17 mmol) in dry DMF (20 mL) was degassed to remove oxygen and was then heated at 85° C. under a blanket of nitrogen for 6.5 hours. Th...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Nitrile
c1ccccc1
c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
Br-
[Zn].[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1
85
null
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21>[Zn].[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-13dc986b879a4a4e809552b5902f8974
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cc(Br)cs1>>CC1(C)OC(=O)Nc2ccc(-c3csc(C#N)c3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC=1C=C(SC1)C#N>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(SC2)C#N)C
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:20]([cH:19]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][s:14][c:15]([C:16]#[N:17])[cH:18]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][s:14][c:15]([C:16]#[N:17])[cH:18]3)[cH:19][c:20]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cc(Br)cs1
CC1(C)OC(=O)Nc2ccc(-c3csc(C#N)c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0b5bebfae8e49ed7172cda779db0d9a1ee34897b702e6169adb1825468a1d911
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccsc3)cc2CO1
Br-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4](-[C:5]#[N;D1;H0:6]):[c:7]:1.O-B(-O)-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]>>[N;D1;H0:6]#[C:5]-[c:4]1:[#16;a:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]):[c:7]:1
null
[]
null
null
null
null
The product was prepared, from (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and 4-bromo-2-thiophenecarbonitrile according to the procedure outlined in Example 5, as a yellowish solid: mp 230–231° C. (decomposed); 1H-NMR (CDCl3) δ 8.32 (s, 1H, D2O exchangeable), 7.83 (d, 1H, J=1.5 Hz), 7.61 (d, 1H...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccsc1
c1ccc2c(c1)COCN2.c1ccsc1
c1ccc2c(c1)COCN2.c1ccsc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cc(Br)cs1>>CC1(C)OC(=O)Nc2ccc(-c3csc(C#N)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a23622732e894873b8b5a7d3d74e9251
CC1(C)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(-c3cccc(Cl)c3)cc21
ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=O)C=C1.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=S)C=C1
O=[C:5]1[O:4][C:2]([CH3:1])([CH3:3])[c:20]2[c:8]([cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([Cl:17])[cH:18]3)[cH:19]2)[NH:7]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:6])S2)cc1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[S:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([Cl:17])[cH:18]3)[cH:19][c:...
CC1(C)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC1(C)OC(=S)Nc2ccc(-c3cccc(Cl)c3)cc21
null
null
CC=1C=CC=CC1C
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3ccccc3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
52.7
[{"value": 52.0, "product": "ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=S)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 52.7, "product": "ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=S)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 6-(3-chlorophenyl)-4,4-dimethyl-1,4-dihydro-benzo[d]-[1,3]oxazin-2-one (0.15 g, 0.5 mmol) and Lawesson's reagent (0.24 g, 0.6 mmol) in anhydrous o-xylene was heated at reflux under nitrogen for 3 hours. The solvent was removed and the residue was purified by a flash chromatography (silica gel, hexane:ethyl...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2.c1ccccc1
Other
CC=1C=CC=CC1C
null
null
CC1(C)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>CC=1C=CC=CC1C>CC1(C)OC(=S)Nc2ccc(-c3cccc(Cl)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-56c70a52190b4d3eaec1cc918d735fd3
CC1(C)OC(=O)Nc2ccc(Br)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(Br)cc21
BrC1=CC2=C(NC(OC2(C)C)=O)C=C1.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>BrC1=CC2=C(NC(OC2(C)C)=S)C=C1
O=[C:5]1[O:4][C:2]([CH3:1])([CH3:3])[c:14]2[c:8]([cH:9][cH:10][c:11]([Br:12])[cH:13]2)[NH:7]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:6])S2)cc1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[S:6])[NH:7][c:8]2[cH:9][cH:10][c:11]([Br:12])[cH:13][c:14]21
CC1(C)OC(=O)Nc2ccc(Br)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC1(C)OC(=S)Nc2ccc(Br)cc21
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccccc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
null
[]
null
null
null
null
The product was prepared, from 6-bromo-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one and Lawesson's reagent using the procedure of Example 9, as a white solid: mp 221–222.5° C.; 1H-NMR (CDCl3) δ 9.38 (s, 1H, D2O exchangeable), 7.42 (dd, 1H, J=8.5, 2.1 Hz), 7.29 (d, 1H, J=2.0 Hz), 6.76 (d, 1H, J=8.4 Hz), 1.76 (s, 6...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2
Other
null
null
null
CC1(C)OC(=O)Nc2ccc(Br)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(Br)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-78d414029c0d443d943cdb207a4e71ef
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21
CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(C#N)C=C(C2)F)C.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>CC1(C2=C(NC(O1)=S)C=CC(=C2)C=2C=C(C#N)C=C(C2)F)C
O=[C:5]1[O:4][C:2]([CH3:1])([CH3:3])[c:22]2[c:8]([cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([F:15])[cH:16][c:17]([C:18]#[N:19])[cH:20]3)[cH:21]2)[NH:7]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:6])S2)cc1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[S:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([F:15])[cH:16][c:17]([C:18]#...
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC1(C)OC(=S)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3ccccc3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
null
[]
null
null
null
null
The product was prepared, from 3-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-benzo[d][1,3]oxazin-6-yl)-5-fluorobenzonitrile and Lawesson's reagent using the procedure of Example 9, as a yellow solid: 248–249° C.; 1H-NMR (DMSO-d6) δ 12.3 (s, 1H), 8.15 (bs, 1H), 8.02 (d, 1H, J=10.48 Hz), 7.85–7.78 (m, 3H), 7.13 (d, 1H, J=8.92 Hz)...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2.c1ccccc1
Other
null
null
null
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c74b12003cc8454a8608e851478103ea
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cccc(Br)c1>>CC1(C)OC(=O)Nc2ccc(-c3cccc(C#N)c3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC=1C=C(C#N)C=CC1.C([O-])([O-])=O.[Na+].[Na+]>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(C#N)C=CC2)C
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:21]([cH:20]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][cH:14][cH:15][c:16]([C:17]#[N:18])[cH:19]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([C:17]#[N:18])[cH:19]3)[cH:20][c:21]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cccc(Br)c1
CC1(C)OC(=O)Nc2ccc(-c3cccc(C#N)c3)cc21
null
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1
O.COCCOC
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
25.2
[{"value": 25.0, "product": "CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(C#N)C=CC2)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 25.2, "product": "CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(C#N)C=CC2)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
A mixture of (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid (2.22 g, 10 mmol), 3-bromobenzonitrile (2.18 g, 12 mmol), tetrakis(triphenylphosphine)palladium (0) (0.6 g, 0.52 mmol), and sodium carbonate (2.2 g, 21 mmol) in a mixture of DME and water (70 mL/15 mL) was degassed to remove the oxygen and...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.O.COCCOC
85
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cccc(Br)c1>C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.O.COCCOC>CC1(C)OC(=O)Nc2ccc(-c3cccc(C#N)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d14ffcd17bd24b77be53296b3e5dd34b
CC1(C)OC(=O)Nc2ccc(-c3cccc(C#N)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(-c3cccc(C#N)c3)cc21
CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(C#N)C=CC2)C.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC.C(C)(=O)OCC>>CC1(C2=C(NC(O1)=S)C=CC(=C2)C=2C=C(C#N)C=CC2)C
O=[C:5]1[O:4][C:2]([CH3:1])([CH3:3])[c:21]2[c:8]([cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([C:17]#[N:18])[cH:19]3)[cH:20]2)[NH:7]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:6])S2)cc1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[S:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([C:17]#[N:18])[cH:19]...
CC1(C)OC(=O)Nc2ccc(-c3cccc(C#N)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC1(C)OC(=S)Nc2ccc(-c3cccc(C#N)c3)cc21
null
null
CC=1C=CC=CC1C
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3ccccc3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
20
[{"value": 20.0, "product": "CC1(C2=C(NC(O1)=S)C=CC(=C2)C=2C=C(C#N)C=CC2)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 19.8, "product": "CC1(C2=C(NC(O1)=S)C=CC(=C2)C=2C=C(C#N)C=CC2)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 3-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-benzo [d][1,3]oxazin-6-yl)-benzonitrile (1 g, 3.6 mmol) and Lawesson's reagent (1.8 g, 4.3 mmol) in o-xylene (30 mL) was heated at reflux overnight. The reaction mixture was cooled to room temperature, poured into ethyl acetate (50 mL) and washed with 1 N HCl (2×20 mL)....
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2.c1ccccc1
Other
CC=1C=CC=CC1C
null
null
CC1(C)OC(=O)Nc2ccc(-c3cccc(C#N)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>CC=1C=CC=CC1C>CC1(C)OC(=S)Nc2ccc(-c3cccc(C#N)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fc3c3df4c19f4d1182851641d7f90a04
N#Cc1cc(-c2cccc(F)c2)ccc1N.N#Cc1cc(Br)ccc1N.OB(O)c1cccc(F)c1>>CC(=O)c1cc(-c2cccc(F)c2)ccc1N.N#Cc1cc(-c2cccc(F)c2)ccc1N
FC=1C=C(C=CC1)B(O)O.NC1=C(C#N)C=C(C=C1)Br.Cl.NC1=C(C=C(C=C1)C1=CC(=CC=C1)F)C#N.C[Mg]Br.C([O-])([O-])=O.[Na+].[Na+]>>NC1=C(C=C(C=C1)C1=CC(=CC=C1)F)C#N.NC1=C(C=C(C=C1)C1=CC(=CC=C1)F)C(C)=O
N#[C:2][c:4]1[cH:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][c:11]([F:12])[cH:13]2)[cH:14][cH:15][c:16]1[NH2:17].Br[c:22]1[cH:21][c:20]([C:19]#[N:18])[c:32]([NH2:33])[cH:31][cH:30]1.OB([OH:3])[c:23]1[cH:24][cH:25][cH:26][c:27]([F:28])[cH:29]1>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][c:11]([F:12])[cH:13]...
N#Cc1cc(-c2cccc(F)c2)ccc1N.N#Cc1cc(Br)ccc1N.OB(O)c1cccc(F)c1
CC(=O)c1cc(-c2cccc(F)c2)ccc1N.N#Cc1cc(-c2cccc(F)c2)ccc1N
null
null
C(C)(=O)OCC.C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
f4400f2c9795d874e2dad9b1d3b5f64074956f5d66c8ad207baffe373e4cd3f5
013308dabb1639b708a9e55ceea7cc7402b5b36b5e63b3b814177d2b4ee80cd3
c1ccc(-c2ccccc2)cc1.c1ccc(-c2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].N#[C;H0;D2;+0:6]-[c:7](:[c:8]):[c:9].O-B(-[OH;D1;+0:10])-[c;H0;D3;+0:11](:[c:12]:[c:13]):[c:14]:[c:15]>>[C;D1;H3:16]-[C;H0;D3;+0:6](=[O;H0;D1;+0:10])-[c:7](:[c:8]):[c:9].[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:11](:[c:12]:[c:13]):[c:14]:[c:15]):[c:4]:[c:5]
43
[{"value": 43.0, "product": "NC1=C(C=C(C=C1)C1=CC(=CC=C1)F)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Amino-3′-fluoro[1,1′-biphenyl]-3-carbonitrile was prepared from 3-fluorophenyl boronic acid and 2-amino-5-bromobenzonitrile according to the procedure of Example 4. A solution of 4-amino-3′-fluoro[1,1′-biphenyl]-3-carbonitrile (6.65 g, 31.3 mmol) in anhydrous THF (100 mL) was treated drop wise at room temperature und...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Nitrile.Boronic acid
Ketone
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
Br-.B
C(C)(=O)OCC.C1CCOC1
null
null
N#Cc1cc(-c2cccc(F)c2)ccc1N.N#Cc1cc(Br)ccc1N.OB(O)c1cccc(F)c1>C(C)(=O)OCC.C1CCOC1>CC(=O)c1cc(-c2cccc(F)c2)ccc1N.N#Cc1cc(-c2cccc(F)c2)ccc1N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-015a9bbf3b544e6eab1c363da5e4cbf6
CC(=O)c1cc(-c2cccc(F)c2)ccc1N>>CC(O)c1cc(-c2cccc(F)c2)ccc1N
S(=O)(=O)([O-])[O-].[NH4+].[NH4+].C(C)(=O)OCC.NC1=C(C=C(C=C1)C1=CC(=CC=C1)F)C(C)=O.[BH4-].[Na+]>>NC1=C(C=C(C=C1)C1=CC(=CC=C1)F)C(C)O
[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][c:11]([F:12])[cH:13]2)[cH:14][cH:15][c:16]1[NH2:17]>>[CH3:1][CH:2]([OH:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][c:11]([F:12])[cH:13]2)[cH:14][cH:15][c:16]1[NH2:17]
CC(=O)c1cc(-c2cccc(F)c2)ccc1N
CC(O)c1cc(-c2cccc(F)c2)ccc1N
null
null
CO
Reduction
Reduction of ketone to secondary alcohol
02790ac194d8bf7ccb13d6247c59412024d87f77d2c906ef7804f021f57d5070
1bd3cd74b454139c0a0068ac0135836499926b274bff569df163210c6c944a89
c1ccc(-c2ccccc2)cc1
[C;D1;H3:1]-[C;H0;D3;+0:2](=[O;H0;D1;+0:3])-[c:4](:[c:5]):[c:6]>>[C;D1;H3:1]-[CH;D3;+0:2](-[OH;D1;+0:3])-[c:4](:[c:5]):[c:6]
67
[{"value": 67.0, "product": "NC1=C(C=C(C=C1)C1=CC(=CC=C1)F)C(C)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 66.5, "product": "NC1=C(C=C(C=C1)C1=CC(=CC=C1)F)C(C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
A solution of 1-(4-amino-3′-fluoro[1,1′-biphenyl]-3-yl)ethanone (3 g, 13 mmol) in anhydrous methanol (60 mL) was then treated at room temperature under nitrogen with sodium borohydride in a portion wise manner. After addition, the reaction mixture was stirred for 4 hours, treated with a saturated solution of aqueous am...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
null
null
c1ccccc1.c1ccccc1
null
CO
null
4
CC(=O)c1cc(-c2cccc(F)c2)ccc1N>CO>CC(O)c1cc(-c2cccc(F)c2)ccc1N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c3c749d7e18a4396a634a5985bdbbed0
CC1OC(=O)Nc2ccc(-c3cccc(F)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1OC(=S)Nc2ccc(-c3cccc(F)c3)cc21
FC=1C=C(C=CC1)C=1C=CC2=C(C(OC(N2)=O)C)C1.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>FC=1C=C(C=CC1)C=1C=CC2=C(C(OC(N2)=S)C)C1
O=[C:4]1[O:3][CH:2]([CH3:1])[c:19]2[c:7]([cH:8][cH:9][c:10](-[c:11]3[cH:12][cH:13][cH:14][c:15]([F:16])[cH:17]3)[cH:18]2)[NH:6]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:5])S2)cc1>>[CH3:1][CH:2]1[O:3][C:4](=[S:5])[NH:6][c:7]2[cH:8][cH:9][c:10](-[c:11]3[cH:12][cH:13][cH:14][c:15]([F:16])[cH:17]3)[cH:18][c:19]21
CC1OC(=O)Nc2ccc(-c3cccc(F)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC1OC(=S)Nc2ccc(-c3cccc(F)c3)cc21
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3ccccc3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
null
[]
null
null
null
null
A solution of 6-(3-fluorophenyl)-4-methyl-1,4-dihydro-2H-3,1-benzoxazin-2-one (0.15 g, 0.58 mmol) in toluene was treated with Lawesson's reagent according to the procedure in example 9 to yield 6-(3-fluorophenyl)-4-methyl-1,4-dihydro-2H-3,1-benzoxazin-2-thione (0.08 g, 50%) as an off-white solid (0.08 g, 50%): mp 173–1...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2.c1ccccc1
Other
C1(=CC=CC=C1)C
null
null
CC1OC(=O)Nc2ccc(-c3cccc(F)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>C1(=CC=CC=C1)C>CC1OC(=S)Nc2ccc(-c3cccc(F)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-009c54948d154e898818fbcb52be95ff
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Cc1cc(C#N)sc1Br>>Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC1=C(C=C(S1)C#N)C>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C2=C(C=C(S2)C#N)C)C
OB(O)[c:9]1[cH:10][cH:11][c:12]2[c:13]([cH:14]1)[C:15]([CH3:16])([CH3:17])[O:18][C:19](=[O:20])[NH:21]2.Br[c:8]1[c:2]([CH3:1])[cH:3][c:4]([C:5]#[N:6])[s:7]1>>[CH3:1][c:2]1[cH:3][c:4]([C:5]#[N:6])[s:7][c:8]1-[c:9]1[cH:10][cH:11][c:12]2[c:13]([cH:14]1)[C:15]([CH3:16])([CH3:17])[O:18][C:19](=[O:20])[NH:21]2
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Cc1cc(C#N)sc1Br
Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0b5bebfae8e49ed7172cda779db0d9a1ee34897b702e6169adb1825468a1d911
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3cccs3)cc2CO1
Br-[c;H0;D3;+0:1]1:[#16;a:2]:[c:3]:[c:4]:[c:5]:1-[C;D1;H3:6].O-B(-O)-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:10]:[c:11]>>[C;D1;H3:6]-[c:5]1:[c:4]:[c:3]:[#16;a:2]:[c;H0;D3;+0:1]:1-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:10]:[c:11]
null
[]
null
null
null
null
5-(4,4-Dimethyl-2-oxo-1,4-dihydro-2H-benzo[d][1,3]oxazin-6-yl)-4-methyl-thiophene-2-carbonitrile was prepared, according to the procedure in Example 5 using (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and 5-bromo-4-methyl-2-thiophenecarbonitrile, as an off-white solid: mp 195–200° C.; 1H-NMR (DM...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccsc1
c1ccsc1.c1ccc2c(c1)COCN2
c1ccsc1.c1ccc2c(c1)COCN2
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Cc1cc(C#N)sc1Br>>Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ab8530a118334e6b91e2f78ad5b520fd
COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1.Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=O)N2>>Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
CC1(OC(NC2=C1C=C(C=C2)C2=C(C=C(S2)C#N)C)=O)C.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>CC1(OC(NC2=C1C=C(C=C2)C2=C(C=C(S2)C#N)C)=S)C
COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:20])S2)cc1.O=[C:19]1[O:18][C:15]([CH3:16])([CH3:17])[c:13]2[c:12]([cH:11][cH:10][c:9](-[c:8]3[c:2]([CH3:1])[cH:3][c:4]([C:5]#[N:6])[s:7]3)[cH:14]2)[NH:21]1>>[CH3:1][c:2]1[cH:3][c:4]([C:5]#[N:6])[s:7][c:8]1-[c:9]1[cH:10][cH:11][c:12]2[c:13]([cH:14]1)[C:15]([CH3:16])([CH3:17])[O:18][C:1...
COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1.Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3cccs3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
51.6
[{"value": 46.0, "product": "CC1(OC(NC2=C1C=C(C=C2)C2=C(C=C(S2)C#N)C)=S)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 51.6, "product": "CC1(OC(NC2=C1C=C(C=C2)C2=C(C=C(S2)C#N)C)=S)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 5-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)-4-methylthiophene-2-carbonitrile (5 g, 16.7 mmol) in anhydrous toluene was added, at room temperature under a blanket of nitrogen, Lawesson's reagent (6 g, 14.8 mmol). The reaction mixture was heated at reflux for 2 hrs, allowed to cool to room ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccccc1.P1SPS1.c1ccccc1.c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2
c1ccsc1.c1ccc2c(c1)COCN2
Other
C1(=CC=CC=C1)C
null
null
COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1.Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=O)N2>C1(=CC=CC=C1)C>Cc1cc(C#N)sc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-db15c1f0a4b242c197627609f45b94e7
CC(C)(C)OC(=O)n1cccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.O=C=NS(=O)(=O)Cl>>CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
O.CN(C)C=O.C(C)(C)(C)OC(=O)N1C(=CC=C1)C1=CC2=C(NC(OC2(C)C)=O)C=C1.ClS(=O)(=O)N=C=O>>C(C)(C)(C)OC(=O)N1C(=CC=C1C#N)C1=CC2=C(NC(OC2(C)C)=O)C=C1
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[n:8]1[cH:9][cH:12][cH:13][c:14]1-[c:15]1[cH:16][cH:17][c:18]2[c:19]([cH:20]1)[C:21]([CH3:22])([CH3:23])[O:24][C:25](=[O:26])[NH:27]2.O=S(=O)(Cl)[N:11]=[C:10]=O>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[n:8]1[c:9]([C:10]#[N:11])[cH:12][cH:13][c:14]1-[c:15]1[cH:16]...
CC(C)(C)OC(=O)n1cccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.O=C=NS(=O)(=O)Cl
CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
null
null
C1CCOC1
C-C Coupling
OtherReaction
93891aa133e496a7c8d865002378d802d0a23f0a704cdcc3cfb3ca39bcb75312
b8bacb90390718f4555f6dee24489036b4f724075b0543a5a9bf8e9abad9b32c
O=C1Nc2ccc(-c3ccc[nH]3)cc2CO1
Cl-S(=O)(=O)-[N;H0;D2;+0:1]=[C;H0;D2;+0:2]=O.[C;D1;H3:3]-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[#8:7]-[C:8](=[O;D1;H0:9])-[#7;a:10]1:[c:11]:[c:12]:[c:13]:[cH;D2;+0:14]:1>>[C;D1;H3:3]-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[#8:7]-[C:8](=[O;D1;H0:9])-[#7;a:10]1:[c:11]:[c:12]:[c:13]:[c;H0;D3;+0:14]:1-[C;H0;D2;+0:2]#[N;H0;D1;+0:1]
52
[{"value": 52.0, "product": "C(C)(C)(C)OC(=O)N1C(=CC=C1C#N)C1=CC2=C(NC(OC2(C)C)=O)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 51.6, "product": "C(C)(C)(C)OC(=O)N1C(=CC=C1C#N)C1=CC2=C(NC(OC2(C)C)=O)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
90
MINUTE
To a solution of 2-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-benzo [d][1,3]oxazin-6-yl)-pyrrole-1-carboxylic acid tert-butyl ester (2.0 g, 5.8 mmol) in THF (anhydrous, 50 mL) at −78° C. was added chlorosulfonyl isocyanate (0.66 mL, 6.7 mmol). After 90 min, DMF (9 mL, 116 mmol) was added and the reaction was allowed to warm to...
10.6084/m9.figshare.5104873.v1
null
null
Nitrile
c1ccc[nH]1
c1ccc[nH]1
c1ccc[nH]1.c1ccc2c(c1)COCN2
HCl
C1CCOC1
null
1.5
CC(C)(C)OC(=O)n1cccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.O=C=NS(=O)(=O)Cl>C1CCOC1>CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4ff7fa3e145d4def93231e90d3a108d9
CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
C(C)(C)(C)OC(=O)N1C(=CC=C1C#N)C1=CC2=C(NC(OC2(C)C)=O)C=C1.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>C(#N)C=1N(C(=CC1)C=1C=CC2=C(C(OC(N2)=S)(C)C)C1)C(=O)OC(C)(C)C
O=[C:25]1[O:24][C:21]([CH3:22])([CH3:23])[c:19]2[c:18]([cH:17][cH:16][c:15](-[c:14]3[n:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[c:9]([C:10]#[N:11])[cH:12][cH:13]3)[cH:20]2)[NH:27]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:26])S2)cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[n:8]1[c:9]([C:10]#[N:11])[cH:12...
CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3ccc[nH]3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
38
[{"value": 38.0, "product": "C(#N)C=1N(C(=CC1)C=1C=CC2=C(C(OC(N2)=S)(C)C)C1)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 34.1, "product": "C(#N)C=1N(C(=CC1)C=1C=CC2=C(C(OC(N2)=S)(C)C)C1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
To 2-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-benzo [d][1,3]oxazin-6-yl)-5-cyano-pyrrole-1-carboxylic acid tert-butyl ester (1.3 g, 35 mmol, 1 eq) in toluene (130 mL) was added Lawesson's reagent (1.58 g, 3.9 mmol, 1.1 eq) and the reaction mixture was heated to 80° C. for 2 h. The solvent was removed in vacuo and the residue...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc[nH]1.c1ccc2c(c1)COCN2
Other
C1(=CC=CC=C1)C
80
null
CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>C1(=CC=CC=C1)C>CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6015e02f55894b85954ab8a8d7c24322
CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2>>CC1(C)OC(=S)Nc2ccc(-c3ccc(C#N)[nH]3)cc21
C(#N)C=1N(C(=CC1)C=1C=CC2=C(C(OC(N2)=S)(C)C)C1)C(=O)OC(C)(C)C.CC[O-].[Na+]>>CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2)C#N)=S)C
CC(C)(C)OC(=O)[n:18]1[c:12](-[c:11]2[cH:10][cH:9][c:8]3[c:20]([cH:19]2)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[S:6])[NH:7]3)[cH:13][cH:14][c:15]1[C:16]#[N:17]>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[S:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([C:16]#[N:17])[nH:18]3)[cH:19][c:20]21
CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
CC1(C)OC(=S)Nc2ccc(-c3ccc(C#N)[nH]3)cc21
null
null
CCO.C1CCOC1
Reduction
Boc amine deprotection
252fa31ad5d8c65b4b59e02901526a39d1fe6cc2afabebaaa627f6f163db1fda
e1bf5a54b1f87284564f107662531aec2aff7de801e4606340967b38924afb28
S=C1Nc2ccc(-c3ccc[nH]3)cc2CO1
C-C(-C)(-C)-O-C(=O)-[n;H0;D3;+0:1]1:[c:2](-[c:3]):[c:4]:[c:5]:[c:6]:1-[C:7]#[N;D1;H0:8]>>[N;D1;H0:8]#[C:7]-[c:6]1:[c:5]:[c:4]:[c:2](-[c:3]):[nH;D2;+0:1]:1
73.3
[{"value": 73.0, "product": "CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2)C#N)=S)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73.3, "product": "CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2)C#N)=S)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
To a solution of tert-butyl 2-cyano-5-(4,4-dimethyl-2-thioxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)-1H-pyrrole-1-carboxylate (0.5 g, 1.3 mmol, 1 eq) in THF (5 mL) was added NaOEt (0.27 g, 3.9 mmol, 3 eq) in EtOH (5 mL) and the reaction was heated to 80° C. for 2 h. The solvents were removed in vacuo and the residue partit...
10.6084/m9.figshare.5104873.v1
null
Ether.Boc
null
c1ccc[nH]1
c1cc[nH]c1
c1ccc2c(c1)COCN2.c1cc[nH]c1
HO-
CCO.C1CCOC1
80
null
CC(C)(C)OC(=O)n1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2>CCO.C1CCOC1>CC1(C)OC(=S)Nc2ccc(-c3ccc(C#N)[nH]3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4ea1fcb9fde041f49e9ca6d730038d52
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#CCc1cccc(Br)n1>>CC1(C)OC(=O)Nc2ccc(-c3cccc(CC#N)n3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC1=CC=CC(=N1)CC#N>>CC1(OC(NC2=C1C=C(C=C2)C2=CC=CC(=N2)CC#N)=O)C
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:22]([cH:21]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][cH:14][cH:15][c:16]([CH2:17][C:18]#[N:19])[n:20]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([CH2:17][C:18]#[N:19])[n:20]3)[cH:21][c:22]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#CCc1cccc(Br)n1
CC1(C)OC(=O)Nc2ccc(-c3cccc(CC#N)n3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
c51c4a152462d99e6f839fd7f446f3100033003c41266a5cf8db98a2232a1323
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccn3)cc2CO1
Br-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:5]:[c:4]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[#7;a:2]:[c:3]
null
[]
null
null
null
null
[6-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)pyridin-2-yl]acetonitrile was prepared, according to the procedure of Example 5 using (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and (6-bromo-2-pyridyl)acetonitrile (J. Org. Chem. 1988, 53, 786–790), as an off-white solid: mp 210–212.5° ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccncc1
c1ccc2c(c1)COCN2.c1ccncc1
c1ccc2c(c1)COCN2.c1ccncc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#CCc1cccc(Br)n1>>CC1(C)OC(=O)Nc2ccc(-c3cccc(CC#N)n3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-177a096a64d244cd9238a2669e7e79fc
CC1(C)OC(=O)Nc2ccc(-c3cccc(CC#N)n3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(-c3cccc(CC#N)n3)cc21
CC1(OC(NC2=C1C=C(C=C2)C2=CC=CC(=N2)CC#N)=O)C.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>CC1(OC(NC2=C1C=C(C=C2)C2=CC=CC(=N2)CC#N)=S)C
O=[C:5]1[O:4][C:2]([CH3:1])([CH3:3])[c:22]2[c:8]([cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([CH2:17][C:18]#[N:19])[n:20]3)[cH:21]2)[NH:7]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:6])S2)cc1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[S:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([CH2:17][C:18]...
CC1(C)OC(=O)Nc2ccc(-c3cccc(CC#N)n3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC1(C)OC(=S)Nc2ccc(-c3cccc(CC#N)n3)cc21
null
null
CC=1C=CC(=CC1)C
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3ccccn3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
92.3
[{"value": 48.0, "product": "CC1(OC(NC2=C1C=C(C=C2)C2=CC=CC(=N2)CC#N)=S)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.3, "product": "CC1(OC(NC2=C1C=C(C=C2)C2=CC=CC(=N2)CC#N)=S)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To [6-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)pyridin-2-yl]acetonitrile (80 mg, 0.27 mmol, 1 eq) in p-xylene (10 mL) was added Lawesson's reagent (55 mg, 0.14 mmol, 0.5 eq) and the reaction was heated to reflux for 2 hours. The reaction was cooled to room temperature and adsorbed onto silica gel. Purific...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2.c1ccncc1
Other
CC=1C=CC(=CC1)C
null
null
CC1(C)OC(=O)Nc2ccc(-c3cccc(CC#N)n3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>CC=1C=CC(=CC1)C>CC1(C)OC(=S)Nc2ccc(-c3cccc(CC#N)n3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ecc1c2e24f1b4386b9eb3ea4bd1f9cc0
CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)[nH]3)cc21.CI>>Cn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
O.IC.CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2)C#N)=O)C.C([O-])([O-])=O.[K+].[K+]>>CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2C)C#N)=O)C
[nH:2]1[c:3]([C:4]#[N:5])[cH:6][cH:7][c:8]1-[c:9]1[cH:10][cH:11][c:12]2[c:13]([cH:14]1)[C:15]([CH3:16])([CH3:17])[O:18][C:19](=[O:20])[NH:21]2.I[CH3:1]>>[CH3:1][n:2]1[c:3]([C:4]#[N:5])[cH:6][cH:7][c:8]1-[c:9]1[cH:10][cH:11][c:12]2[c:13]([cH:14]1)[C:15]([CH3:16])([CH3:17])[O:18][C:19](=[O:20])[NH:21]2
CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)[nH]3)cc21.CI
Cn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
3b0bd5806650bb387428bf36a5e436078e57d40d2afdf9e751829e2a02da9e1d
7a358c636daddc97c1fb4c29f378044d7eac3f01815d9966e599841f642d631a
O=C1Nc2ccc(-c3ccc[nH]3)cc2CO1
I-[CH3;D1;+0:1].[N;D1;H0:2]#[C:3]-[c:4]1:[c:5]:[c:6]:[c:7](-[c:8]):[nH;D2;+0:9]:1>>[CH3;D1;+0:1]-[n;H0;D3;+0:9]1:[c:4](-[C:3]#[N;D1;H0:2]):[c:5]:[c:6]:[c:7]:1-[c:8]
41
[{"value": 41.0, "product": "CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2C)C#N)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 39.5, "product": "CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2C)C#N)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a solution of 5-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)-1H-pyrrole-2-carbonitrile (1 eq, 71 mg, 0.27 mmol) in dimethylformamide (0.5 mL) was added potassium carbonate (5 eq, 0.18 g, 0.1.35 mmol). After 10 min, iodomethane (3 eq, 0.05 mL, 0.81 mmol) was added and the suspension was stirred for 2 hours...
10.6084/m9.figshare.5104873.v1
null
null
null
c1cc[nH]c1
c1ccc[nH]1
c1ccc[nH]1.c1ccc2c(c1)COCN2
HI
CN(C=O)C
null
0.166667
CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)[nH]3)cc21.CI>CN(C=O)C>Cn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e8794b502b524658ab1f47d116081e3c
CC1(C)OC(=O)Nc2ccc(-c3cc(C#N)cs3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(-c3cc(C#N)cs3)cc21
CC1(C2=C(NC(O1)=O)C=CC(=C2)C2=CC(=CS2)C#N)C.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>CC1(C2=C(NC(O1)=S)C=CC(=C2)C2=CC(=CS2)C#N)C
O=[C:5]1[O:4][C:2]([CH3:1])([CH3:3])[c:20]2[c:8]([cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([C:15]#[N:16])[cH:17][s:18]3)[cH:19]2)[NH:7]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:6])S2)cc1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[S:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([C:15]#[N:16])[cH:17][s:18]3)[cH:19][c:20]2...
CC1(C)OC(=O)Nc2ccc(-c3cc(C#N)cs3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC1(C)OC(=S)Nc2ccc(-c3cc(C#N)cs3)cc21
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3cccs3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
null
[]
null
null
null
null
The title compound was prepared in a manner similar to Example 16 using 5-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-benzo [d][1,3]oxazin-6-yl) thiophene-3-carbonitrile and Lawesson's reagent. The product was obtained in the form of yellow crystals: m.p. 258–259° C. 1H NMR (DMSO-d6) δ 12.3 (s, 1 H), 8.54 (d, 1H, J=0.9 Hz), 7.9...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2.c1ccsc1
Other
O
null
null
CC1(C)OC(=O)Nc2ccc(-c3cc(C#N)cs3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>O>CC1(C)OC(=S)Nc2ccc(-c3cc(C#N)cs3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-26f4d3e740fb416bb2f637f77eb85032
CCn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CCn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2CC)C#N)=O)C.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>CC1(OC(NC2=C1C=C(C=C2)C2=CC=C(N2CC)C#N)=S)C
O=[C:20]1[O:19][C:16]([CH3:17])([CH3:18])[c:14]2[c:13]([cH:12][cH:11][c:10](-[c:9]3[n:3]([CH2:2][CH3:1])[c:4]([C:5]#[N:6])[cH:7][cH:8]3)[cH:15]2)[NH:22]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:21])S2)cc1>>[CH3:1][CH2:2][n:3]1[c:4]([C:5]#[N:6])[cH:7][cH:8][c:9]1-[c:10]1[cH:11][cH:12][c:13]2[c:14]([cH:15]1)[C:16]([CH3:17])([...
CCn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CCn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3ccc[nH]3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
null
[]
null
null
null
null
The title compound was prepared according to the procedure for Example 16 from 5-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)-1-ethyl-1H-pyrrole-2-carbonitrile and Lawesson's reagent. The product was obtained in the form of white needles: mp 212–213° C.; 1H-NMR (DMSO-d6) δ 1.25 (t, 3H, J-=7 Hz), 1.68 (s, 6H)...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc[nH]1.c1ccc2c(c1)COCN2
Other
null
null
null
CCn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=O)N2.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CCn1c(C#N)ccc1-c1ccc2c(c1)C(C)(C)OC(=S)N2
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1b0ec4d5d2d24b0a8fad1554ad70fa06
BrCCCCCBr.Nc1ccc(Br)cc1C(=O)O>>Nc1ccc(Br)cc1C1(O)CCCCC1
NC1=C(C(=O)O)C=C(C=C1)Br.BrCCCCCBr>>NC1=C(C=C(C=C1)Br)C1(CCCCC1)O
Br[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]Br.O=[C:9]([c:8]1[c:2]([NH2:1])[cH:3][cH:4][c:5]([Br:6])[cH:7]1)[OH:10]>>[NH2:1][c:2]1[cH:3][cH:4][c:5]([Br:6])[cH:7][c:8]1[C:9]1([OH:10])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]1
BrCCCCCBr.Nc1ccc(Br)cc1C(=O)O
Nc1ccc(Br)cc1C1(O)CCCCC1
null
null
null
C-C Coupling
OtherReaction
9e5c378844480bc1e13d9f9ac0348ea73b576c5d624749e5b7c271d467b79866
822e973608b3f0d7a885c0b5584a307ebd92fa7f731ed8882df7c309f292b5c4
c1ccc(C2CCCCC2)cc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]-[CH2;D2;+0:5]-Br.O=[C;H0;D3;+0:6](-[O;D1;H1:7])-[c:8](:[c:9]):[c:10]>>[O;D1;H1:7]-[C;H0;D4;+0:6]1(-[c:8](:[c:9]):[c:10])-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]-[CH2;D2;+0:5]-1
null
[]
null
null
null
null
1-(2-Amino-5-bromo-phenyl) cyclohexanol was prepared, according to the procedure of Example 1 using 2-amino-5-bromobenzoic acid and the Grignard reagent prepared from 1,5-dibromopentane, as a clear oil: 1H-NMR (DMSO-d6) δ 7.07 (d, 1H, J=2.3 Hz), 7.03 (dd, 1H, J=8.4, 2.4 Hz), 6.55 (d, 1H, J=8.6 Hz), 5.49 (s, 2H, D2O exc...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Carboxylic acid
Tertiary alcohol
null
C1CCCCC1
c1ccccc1.C1CCCCC1
Br-
null
null
null
BrCCCCCBr.Nc1ccc(Br)cc1C(=O)O>>Nc1ccc(Br)cc1C1(O)CCCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-387f011555704388b9d4a17550cb3977
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Cc1cc(Br)cc(Br)c1>>Cc1cc(Br)cc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC=1C=C(C=C(C1)Br)C>>BrC=1C=C(C=C(C1)C)C1=CC2=C(NC(OC2(C)C)=O)C=C1
OB(O)[c:8]1[cH:9][cH:10][c:11]2[c:12]([cH:13]1)[C:14]([CH3:15])([CH3:16])[O:17][C:18](=[O:19])[NH:20]2.Br[c:7]1[cH:6][c:4]([Br:5])[cH:3][c:2]([CH3:1])[cH:21]1>>[CH3:1][c:2]1[cH:3][c:4]([Br:5])[cH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]3[c:12]([cH:13]2)[C:14]([CH3:15])([CH3:16])[O:17][C:18](=[O:19])[NH:20]3)[cH:21]1
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Cc1cc(Br)cc(Br)c1
Cc1cc(Br)cc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:10]:[c:9]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:7]:[c:8]
null
[]
null
null
null
null
6-(3-Bromo-5-methyl-phenyl)-4,4-dimethyl-1,4-dihydrobenzo-[d][1,3]oxazin-2-one was prepared, using (4,4-dimethyl-1,4-dihydro-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and 3,5-dibromotoluene according to the procedure of Example 5, as a white solid: mp 231–233° C.; 1H-NMR (DMSO-d6) δ 10.4 (s, 1H), 7.66 (s, 1H), 7.58–7.5...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccccc1.c1ccc2c(c1)COCN2
c1ccccc1.c1ccc2c(c1)COCN2
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Cc1cc(Br)cc(Br)c1>>Cc1cc(Br)cc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-09cddcd17bf84b12b7190e0584d9b2ef
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.FC(F)(F)Oc1cc(Br)cc(Br)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(Br)cc(OC(F)(F)F)c3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC1=CC(=CC(=C1)OC(F)(F)F)Br>>BrC=1C=C(C=C(C1)OC(F)(F)F)C1=CC2=C(NC(OC2(C)C)=O)C=C1
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:25]([cH:24]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][c:14]([Br:15])[cH:16][c:17]([O:18][C:19]([F:20])([F:21])[F:22])[cH:23]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([Br:15])[cH:16][c:17]([O:18][C:19]([F:20...
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.FC(F)(F)Oc1cc(Br)cc(Br)c1
CC1(C)OC(=O)Nc2ccc(-c3cc(Br)cc(OC(F)(F)F)c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
null
[]
null
null
null
null
6-(3-Bromo-5-trifluoromethoxy-phenyl)-4,4-dimethyl-1,4-dihydrobenzo [d][1,3]-oxazin-2-one was prepared, using (4,4-dimethyl-1,4-dihydro-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and 1, 3-dibromo-5-trifluoromethoxybenzene according to the procedure of Example 5, as a white solid: mp 214–216° C.; 1H-NMR (DMSO-d6) δ 10.4 ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.FC(F)(F)Oc1cc(Br)cc(Br)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(Br)cc(OC(F)(F)F)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4c7762fc30dd474b866ea6126d0bc089
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1cc(Cl)cc(Cl)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(Cl)cc(Cl)c3)cc21
BrC1=CC2=C(NC(OC2(C)C)=O)C=C1.ClC=1C=C(C=C(C1)Cl)B(O)O>>ClC=1C=C(C=C(C1)Cl)C1=CC2=C(NC(OC2(C)C)=O)C=C1
Br[c:11]1[cH:10][cH:9][c:8]2[c:21]([cH:20]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.OB(O)[c:12]1[cH:13][c:14]([Cl:15])[cH:16][c:17]([Cl:18])[cH:19]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([Cl:15])[cH:16][c:17]([Cl:18])[cH:19]3)[cH:20][c:21]21
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1cc(Cl)cc(Cl)c1
CC1(C)OC(=O)Nc2ccc(-c3cc(Cl)cc(Cl)c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:8]:[c:7]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:9]:[c:10]
null
[]
null
null
null
null
6-(3,5-dichloro-phenyl)-4,4-dimethyl-1,4-dihydrobenzo-[d][1,3]oxazin-2-one was prepared, from 6-bromo-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one and 3,5-dichlorophenyl boronic acid according to the procedure of Example 4, as a white solid: mp 245–246° C.; 1H-NMR (DMSO-d6) δ 10.4 (s, 1H), 7.77 (m, 2H), 7.67–7.64...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1cc(Cl)cc(Cl)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(Cl)cc(Cl)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3a27f1abc1d34ba6aba1da24b87462ad
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1ccc(Br)o1>>CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)o3)cc21
BrC=1OC(=CC1)C#N.CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C2=CC=C(O2)C#N)C
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:20]([cH:19]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][cH:14][c:15]([C:16]#[N:17])[o:18]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([C:16]#[N:17])[o:18]3)[cH:19][c:20]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1ccc(Br)o1
CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)o3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
4f7d7b24f806b5cd4e85a32312d9881a35e9e6beb03f90f98c00ef7f864a3ecf
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccco3)cc2CO1
Br-[c;H0;D3;+0:1]1:[#8;a:2]:[c:3]:[c:4]:[c:5]:1.O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:10]:[c:9]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1]1:[#8;a:2]:[c:3]:[c:4]:[c:5]:1):[c:7]:[c:8]
null
[]
null
null
null
null
5-(4,4-Dimethyl-2-oxo-1,4-dihydro-2H-benzo[d][1,3]oxazin-6-yl)-furan-2-carbonitrile was prepared, according to the procedure of Example 5 from 2-bromo-5-cyanofuran (1.0 g, 5.6 mmol) (J. Med. Chem. (1997), 40(23), 3804–3819) and (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid (1.8 g, 8.18 mmol), as a...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccoc1
c1ccc2c(c1)COCN2.c1ccoc1
c1ccc2c(c1)COCN2.c1ccoc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1ccc(Br)o1>>CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)o3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0c428ae268674c619645cd09cab52c13
CCC1(CC)OC(=O)Nc2ccc(I)cc21.O=[N+]([O-])c1cccc(B(O)O)c1>>CCC1(CC)OC(=O)Nc2ccc(-c3cccc([N+](=O)[O-])c3)cc21
C(C)C1(C2=C(NC(O1)=O)C=CC(=C2)I)CC.[N+](=O)([O-])C=1C=C(C=CC1)B(O)O>>C(C)C1(C2=C(NC(O1)=O)C=CC(=C2)C2=CC(=CC=C2)[N+](=O)[O-])CC
I[c:13]1[cH:12][cH:11][c:10]2[c:24]([cH:23]1)[C:3]([CH2:2][CH3:1])([CH2:4][CH3:5])[O:6][C:7](=[O:8])[NH:9]2.OB(O)[c:14]1[cH:15][cH:16][cH:17][c:18]([N+:19](=[O:20])[O-:21])[cH:22]1>>[CH3:1][CH2:2][C:3]1([CH2:4][CH3:5])[O:6][C:7](=[O:8])[NH:9][c:10]2[cH:11][cH:12][c:13](-[c:14]3[cH:15][cH:16][cH:17][c:18]([N+:19](=[O:20...
CCC1(CC)OC(=O)Nc2ccc(I)cc21.O=[N+]([O-])c1cccc(B(O)O)c1
CCC1(CC)OC(=O)Nc2ccc(-c3cccc([N+](=O)[O-])c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
I-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
null
[]
null
null
null
null
4,4-Diethyl-6-(3-nitrophenyl)-1,4-dihydrobenzo[d][1,3]oxazin-2-one was prepared, from 4,4-diethyl-6-iodo-1,4-dihydrobenzo[d][1,3]oxazin-2-one and 3-nitrophenyl boronic acid according to the procedure of Example 4, as an off-white solid: mp 193–194° C.; 1H-NMR (CDCl3) δ 9.19 (s, 1H, D2O exchangeable), 8.38 (t, 1H, J=1.9...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HI.B
null
null
null
CCC1(CC)OC(=O)Nc2ccc(I)cc21.O=[N+]([O-])c1cccc(B(O)O)c1>>CCC1(CC)OC(=O)Nc2ccc(-c3cccc([N+](=O)[O-])c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6ff33a7f98944b36839c5de267a2d46a
CON(C)C(=O)c1cc(Br)ccc1N.OB(O)c1cccc(Cl)c1>>CON(C)C(=O)c1cccc(-c2cccc(Cl)c2)c1
NC1=C(C(=O)N(C)OC)C=C(C=C1)Br.ClC=1C=C(C=CC1)B(O)O.C([O-])([O-])=O.[Na+].[Na+]>>ClC=1C=C(C=CC1)C=1C=CC=C(C(=O)N(C)OC)C1
N[c:8]1[c:7]([C:5]([N:3]([O:2][CH3:1])[CH3:4])=[O:6])[cH:19][c:11](Br)[cH:10][cH:9]1.OB(O)[c:12]1[cH:13][cH:14][cH:15][c:16]([Cl:17])[cH:18]1>>[CH3:1][O:2][N:3]([CH3:4])[C:5](=[O:6])[c:7]1[cH:8][cH:9][cH:10][c:11](-[c:12]2[cH:13][cH:14][cH:15][c:16]([Cl:17])[cH:18]2)[cH:19]1
CON(C)C(=O)c1cc(Br)ccc1N.OB(O)c1cccc(Cl)c1
CON(C)C(=O)c1cccc(-c2cccc(Cl)c2)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
O.COCCOC
C-C Coupling
OtherReaction
935af4259c4975cac487da8e9b2dade0b8df326796e05a95adf1d4d492f1807a
79fc43732b29814f22dd0a7cbc24a0ef705cb8e808911cfb2a64a2630fa44903
c1ccc(-c2ccccc2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c;H0;D3;+0:4](-N):[c:5](-[C:6](=[O;D1;H0:7])-[#7:8](-[#8:9])-[C;D1;H3:10]):[c:11]:1.O-B(-O)-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[#8:9]-[#7:8](-[C;D1;H3:10])-[C:6](=[O;D1;H0:7])-[c:5]1:[c:11]:[c;H0;D3;+0:1](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]):[c:2]:[c:3]:[cH;D2;+0:4...
60.4
[{"value": 57.0, "product": "ClC=1C=C(C=CC1)C=1C=CC=C(C(=O)N(C)OC)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 60.4, "product": "ClC=1C=C(C=CC1)C=1C=CC=C(C(=O)N(C)OC)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
A mixture of 2-amino-5-bromo-N-methoxy-N-methylbenzamide (7.78 g, 30 mmol), 3-chlorophenyl boronic acid (5.63 g, 36 mmol), tetrakis(triphenylphosphine)palladium (0) (1.73 g, 1.5 mmol), and sodium carbonate (7.63 g, 72 mmol) in a mixture of DME and water (150 mL/30 mL) was degassed to remove the oxygen and heated at 85°...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine.Boronic acid
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
HBr.B
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.O.COCCOC
85
null
CON(C)C(=O)c1cc(Br)ccc1N.OB(O)c1cccc(Cl)c1>C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.O.COCCOC>CON(C)C(=O)c1cccc(-c2cccc(Cl)c2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-eb2f155c4449479dbc7f4fd79ec84839
CON(C)C(=O)c1cccc(-c2cccc(Cl)c2)c1.[NH4+]>>CC(=O)c1cc(-c2cccc(Cl)c2)ccc1N
C(C)(=O)OCC.ClC=1C=C(C=CC1)C=1C=CC=C(C(=O)N(C)OC)C1.C[Li].[Cl-].[NH4+]>>NC1=C(C=C(C=C1)C1=CC(=CC=C1)Cl)C(C)=O
CON(C)[C:2](=[O:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][c:11]([Cl:12])[cH:13]2)[cH:14][cH:15][cH:16]1.[NH4+:17]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][c:11]([Cl:12])[cH:13]2)[cH:14][cH:15][c:16]1[NH2:17]
CON(C)C(=O)c1cccc(-c2cccc(Cl)c2)c1.[NH4+]
CC(=O)c1cc(-c2cccc(Cl)c2)ccc1N
null
null
CCOCC.C1CCOC1
C-C Coupling
OtherReaction
d9e625bca5029b45899b727e5c506ae99b3f747ad8055f1c5fc71a14a0c85b03
2fbd26488ea02b131f565aa7b6fdcc6afd5764ffbfd21b2d786b3ac148ebc329
c1ccc(-c2ccccc2)cc1
C-O-N(-C)-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[cH;D2;+0:5]:[c:6]:[c:7].[NH4+;D0:8]>>[C;D1;H3:9]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c;H0;D3;+0:5](-[NH2;D1;+0:8]):[c:6]:[c:7]
47
[{"value": 47.0, "product": "NC1=C(C=C(C=C1)C1=CC(=CC=C1)Cl)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A mixture of 2-amino-5-bromo-N-methoxy-N-methylbenzamide (7.78 g, 30 mmol), 3-chlorophenyl boronic acid (5.63 g, 36 mmol), tetrakis(triphenylphosphine)palladium (0) (1.73 g, 1.5 mmol), and sodium carbonate (7.63 g, 72 mmol) in a mixture of DME and water (150 mL/30 mL) was degassed to remove the oxygen and heated at 85°...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Ketone.Primary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HO-
CCOCC.C1CCOC1
null
0.5
CON(C)C(=O)c1cccc(-c2cccc(Cl)c2)c1.[NH4+]>CCOCC.C1CCOC1>CC(=O)c1cc(-c2cccc(Cl)c2)ccc1N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-32cecf2ca50b4412a37e97546a0bac8c
CC(=O)c1cc(-c2cccc(Cl)c2)ccc1N.O=C(n1ccnc1)n1ccnc1.[Br][Mg][c]1ccccc1>>CC1(c2ccccc2)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
C1CCOC1.NC1=C(C=C(C=C1)C1=CC(=CC=C1)Cl)C(C)=O.C1(=CC=CC=C1)[Mg]Br.C1=CN(C=N1)C(=O)N2C=CN=C2>>ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C2=CC=CC=C2)C)=O)C=C1
[CH3:1][C:2](=[O:9])[c:25]1[c:13]([NH2:12])[cH:14][cH:15][c:16](-[c:17]2[cH:18][cH:19][cH:20][c:21]([Cl:22])[cH:23]2)[cH:24]1.c1cn([C:10](n2ccnc2)=[O:11])cn1.[Br][Mg][c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1>>[CH3:1][C:2]1([c:3]2[cH:4][cH:5][cH:6][cH:7][cH:8]2)[O:9][C:10](=[O:11])[NH:12][c:13]2[cH:14][cH:15][c:16](-[c:17]3...
CC(=O)c1cc(-c2cccc(Cl)c2)ccc1N.O=C(n1ccnc1)n1ccnc1.[Br][Mg][c]1ccccc1
CC1(c2ccccc2)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
null
null
null
C-C Coupling
OtherReaction
f58a792c9a8544457dec510324c5228ba9ef6635800cdc56785c13deeccae300
90008ef043900bdf87d9d5fd1a862da1cc24a9fb439932e381713f7ba0baeb59
O=C1Nc2ccc(-c3ccccc3)cc2C(c2ccccc2)O1
[Br]-[Mg]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[C;D1;H3:6]-[C;H0;D3;+0:7](=[O;H0;D1;+0:8])-[c:9](:[c:10]):[c:11](-[NH2;D1;+0:12]):[c:13].[O;D1;H0:14]=[C;H0;D3;+0:15](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[C;D1;H3:6]-[C;H0;D4;+0:7]1(-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5])-[O;H0;D2;+0:8]-[C;H0;D3;+0:15](=[O;D1;H0:14])-[NH;...
null
[]
null
null
null
null
6-(3-Chlorophenyl)-4-methyl-4-phenyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one was prepared, from 1-(4-amino-3′-chloro-biphenyl-3-yl)-ethanone (0.2 g, 0.82 mmol) and phenylmagnesium bromide followed by treatment with CDI in THF, as a white solid: mp 179–180° C.; 1H-NMR (CDCl3) δ 8.27 (s, 1H, D2O exchangeable), 7.51–7.57 (m...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Ketone.Primary amine
Carbamic ester.Ether
c1c[nH]cn1.c1c[nH]cn1.c1ccccc1
c1ccccc1.c1ccc2c(c1)COCN2
c1ccccc1.c1ccc2c(c1)COCN2.c1ccccc1
HBr.Mg
null
null
null
CC(=O)c1cc(-c2cccc(Cl)c2)ccc1N.O=C(n1ccnc1)n1ccnc1.[Br][Mg][c]1ccccc1>>CC1(c2ccccc2)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-80da410e3a34442a9c0e79cfc16cc22c
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(F)cc(Br)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(F)c3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC1=CC(=CC(=C1)F)F>>FC=1C=C(C=C(C1)F)C1=CC2=C(NC(OC2(C)C)=O)C=C1
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:21]([cH:20]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][c:14]([F:15])[cH:16][c:17]([F:18])[cH:19]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([F:15])[cH:16][c:17]([F:18])[cH:19]3)[cH:20][c:21]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(F)cc(Br)c1
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(F)c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
null
[]
null
null
null
null
6-(3,5-difluoro-phenyl)-4,4-dimethyl-1,4-dihydrobenzo-[d][1,3]oxazin-2-one was prepared, according to the procedure of Example 5 from (4,4-dimethyl-1,4-dihydro-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and 1-bromo-3,5-difluorobenzene, as a white solid: mp 218–219° C.; 1H-NMR (DMSO-d6) δ 10.4 (s, 1H), 7.67–7.65 (m, 2H),...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(F)cc(Br)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(F)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-988638c796ae45c688be965cb9646779
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.COCCOC>>COc1cc(C#N)cc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.C([O-])([O-])=O.[Na+].[Na+].[Br-].[Li+].O.COCCOC>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(C#N)C=C(C2)OC)C
OB(O)[c:10]1[cH:11][cH:12][c:13]2[c:14]([cH:15]1)[C:16]([CH3:17])([CH3:18])[O:19][C:20](=[O:21])[NH:7]2.O([CH2:4][CH2:3][O:2][CH3:1])[CH3:5]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([C:6]#[N:7])[cH:8][c:9](-[c:10]2[cH:11][cH:12][c:13]3[c:14]([cH:15]2)[C:16]([CH3:17])([CH3:18])[O:19][C:20](=[O:21])[NH:22]3)[cH:23]1
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.COCCOC
COc1cc(C#N)cc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
null
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1
C(C)(=O)OCC
Aromatic Heterocycle Formation
OtherReaction
10a74f45bf132ebcc20e108a859f92b7de536fe3d7ed4fb13802789a8f67edab
4216aae7036d4a7562fc0c1d39526975f9f6c0c8a2f5f093a06ee9e8e2e4ca8a
O=C1Nc2ccc(-c3ccccc3)cc2CO1
O-B(-O)-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c;H0;D3;+0:4]2:[c:5](:[c:6]:1)-[C:7]-[#8:8]-[C;H0;D3;+0:9](=[O;D1;H0:10])-[NH;D2;+0:11]-2.[C;D1;H3:12]-[#8:13]-[CH2;D2;+0:14]-[CH2;D2;+0:15]-O-[CH3;D1;+0:16]>>[C;D1;H3:12]-[#8:13]-[c;H0;D3;+0:14]1:[c:17]:[c:18](-[c;H0;D3;+0:1]2:[c:2]:[c:3]:[c;H0;D3;+0:4]3:[c:5](:[c:6]:2)-[C:7]-[#8:8...
53
[{"value": 53.0, "product": "CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(C#N)C=C(C2)OC)C", "details": "PERCENTYIELD", "is_desired": false}]
50
CELSIUS
15
MINUTE
A mixture of (4,4-dimethyl-1,4-dihydro-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid (4.2 g, 19.0 mmol), 3-cyano-5-methoxybenzyltriflate (5.1 g, 19.0 mmol), tetrakis(triphenylphosphine)-palladium (0) (1.1 g, 0.95 mmol), sodium carbonate (4.0 g, 38.0 mmol), lithium bromide (5 g, 57 mmol) in DME (50 mL), and water (25 mL) un...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Boronic acid
Carbamic ester.Ether.Ether.Nitrile
c1ccc2c(c1)COCN2
c1ccccc1.c1ccc2c(c1)COCN2
c1ccccc1.c1ccc2c(c1)COCN2
HO-.B
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(C)(=O)OCC
50
0.25
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.COCCOC>[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(C)(=O)OCC>COc1cc(C#N)cc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b819503bde5e4c3ba949b637dda5ae03
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1ccc(Br)cc1>>CC1(C)OC(=O)Nc2ccc(-c3ccc(F)cc3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC1=CC=C(C=C1)F>>FC1=CC=C(C=C1)C1=CC2=C(NC(OC2(C)C)=O)C=C1
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:20]([cH:19]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][cH:14][c:15]([F:16])[cH:17][cH:18]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([F:16])[cH:17][cH:18]3)[cH:19][c:20]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1ccc(Br)cc1
CC1(C)OC(=O)Nc2ccc(-c3ccc(F)cc3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
null
[]
null
null
null
null
6-(4-Fluoro-phenyl)-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one was prepared, according to the procedure of Example 5 from (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and 1-bromo-4-fluorobenzene, as off-white crystals: mp 232–233° C.; 1H-NMR (DMSO-d6) δ 10.3 (s, 1H), 7.74 (m, 2H), 7.53 (m...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1ccc(Br)cc1>>CC1(C)OC(=O)Nc2ccc(-c3ccc(F)cc3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8e8a22badc9e48b6b9e6dfca240a57f8
BrBr.CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21>>CC1(C)OC(=O)Nc2c(Br)cc(-c3cc(F)cc(C#N)c3)cc21
CC1(OC(NC2=C1C=C(C=C2)C=2C=C(C#N)C=C(C2)F)=O)C.C(C)(=O)[O-].[Na+].BrBr>>BrC1=CC(=CC=2C(OC(NC21)=O)(C)C)C=2C=C(C#N)C=C(C2)F
Br[Br:10].[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:11][c:12](-[c:13]3[cH:14][c:15]([F:16])[cH:17][c:18]([C:19]#[N:20])[cH:21]3)[cH:22][c:23]21>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[c:9]([Br:10])[cH:11][c:12](-[c:13]3[cH:14][c:15]([F:16])[cH:17][c:18]([C:19]#[N:20])[cH:21]3)[cH:22][c...
BrBr.CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21
CC1(C)OC(=O)Nc2c(Br)cc(-c3cc(F)cc(C#N)c3)cc21
null
null
C(C)(=O)O
Functional Group Interconversion
Bromination
f2e1e2237cf85b69b6ca775a9b733eae7076a772fd87c1b40b984f4a2e0b36b9
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[Br;H0;D1;+0:1].[#8:2]-[C:3](=[O;D1;H0:4])-[#7:5]-[c:6](:[c:7]):[cH;D2;+0:8]:[c:9]:[c:10]>>[#8:2]-[C:3](=[O;D1;H0:4])-[#7:5]-[c:6](:[c:7]):[c;H0;D3;+0:8](-[Br;H0;D1;+0:1]):[c:9]:[c:10]
75.3
[{"value": 75.0, "product": "BrC1=CC(=CC=2C(OC(NC21)=O)(C)C)C=2C=C(C#N)C=C(C2)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.3, "product": "BrC1=CC(=CC=2C(OC(NC21)=O)(C)C)C=2C=C(C#N)C=C(C2)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
To a mixture of 3-(4,4-dimethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)-5-fluorobenzonitrile (0.5 g, 1.7 mmol) and sodium acetate (0.2 g, 2.4 mmol) in acetic acid (5 mL) was added, at room temperature under nitrogen, bromine (0.12 mL, 2.34 mmol). The reaction mixture was stirred for 20 hours and then poured into ice ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2.c1ccccc1
HBr
C(C)(=O)O
null
20
BrBr.CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(C#N)c3)cc21>C(C)(=O)O>CC1(C)OC(=O)Nc2c(Br)cc(-c3cc(F)cc(C#N)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-909192587b9c42d1b2da4b6286c124d2
CC1(C)OC(=O)Nc2ccc(I)cc21.O=[N+]([O-])c1cccc(B(O)O)c1>>CC1(C)OC(=O)Nc2ccc(-c3cccc([N+](=O)[O-])c3)cc21
IC1=CC2=C(NC(OC2(C)C)=O)C=C1.[N+](=O)([O-])C=1C=C(C=CC1)B(O)O>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C2=CC(=CC=C2)[N+](=O)[O-])C
I[c:11]1[cH:10][cH:9][c:8]2[c:22]([cH:21]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.OB(O)[c:12]1[cH:13][cH:14][cH:15][c:16]([N+:17](=[O:18])[O-:19])[cH:20]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([N+:17](=[O:18])[O-:19])[cH:20]3)[cH:21][c:22]...
CC1(C)OC(=O)Nc2ccc(I)cc21.O=[N+]([O-])c1cccc(B(O)O)c1
CC1(C)OC(=O)Nc2ccc(-c3cccc([N+](=O)[O-])c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
I-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:8]:[c:7]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:9]:[c:10]
null
[]
null
null
null
null
4,4-Dimethyl-6-(3-nitrophenyl)-1,4-dihydro benzo[d][1,3]oxazin-2-one was prepared, from 6-iodo-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one and 3-nitrophenyl boronic acid according to the procedure of Example 4, as a yellowish solid: mp 244–245° C.; 1H-NMR (DMSO-d6) δ 10.38 (s, 1H, D2O exchangeable), 8.47 (s, 1H)...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HI.B
null
null
null
CC1(C)OC(=O)Nc2ccc(I)cc21.O=[N+]([O-])c1cccc(B(O)O)c1>>CC1(C)OC(=O)Nc2ccc(-c3cccc([N+](=O)[O-])c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-71980f2d95324af0b9651afab633a64f
CCC1(CC)OC(=O)Nc2ccc(I)cc21.OB(O)c1cccc(Cl)c1>>CCC1(CC)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
C(C)C1(C2=C(NC(O1)=O)C=CC(=C2)I)CC.ClC=1C=C(C=CC1)B(O)O>>ClC=1C=C(C=CC1)C1=CC2=C(NC(OC2(CC)CC)=O)C=C1
I[c:13]1[cH:12][cH:11][c:10]2[c:22]([cH:21]1)[C:3]([CH2:2][CH3:1])([CH2:4][CH3:5])[O:6][C:7](=[O:8])[NH:9]2.OB(O)[c:14]1[cH:15][cH:16][cH:17][c:18]([Cl:19])[cH:20]1>>[CH3:1][CH2:2][C:3]1([CH2:4][CH3:5])[O:6][C:7](=[O:8])[NH:9][c:10]2[cH:11][cH:12][c:13](-[c:14]3[cH:15][cH:16][cH:17][c:18]([Cl:19])[cH:20]3)[cH:21][c:22]...
CCC1(CC)OC(=O)Nc2ccc(I)cc21.OB(O)c1cccc(Cl)c1
CCC1(CC)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
I-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
null
[]
null
null
null
null
6-(3-Chlorophenyl)-4,4-diethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one was prepared, from 4,4-diethyl-6-iodo-1,4-dihydrobenzo[d][1,3]oxazin-2-one and 3-chlorophenyl boronic acid according to the procedure of Example 4, as a white solid: mp 150–151° C.; 1H-NMR (CDCl3) δ 8.52 (s, 1H, D2O exchangeable), 7.50 (s, 1H), 7.31–7....
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HI.B
null
null
null
CCC1(CC)OC(=O)Nc2ccc(I)cc21.OB(O)c1cccc(Cl)c1>>CCC1(CC)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cea597d3cda242f9a4a8bf5ab53a4814
CC1(C)OC(=O)Nc2ccc(Br)cc21.COc1cccc(B(O)O)c1>>COc1cccc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
BrC1=CC2=C(NC(OC2(C)C)=O)C=C1.COC=1C=C(C=CC1)B(O)O>>COC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=O)C=C1
Br[c:8]1[cH:9][cH:10][c:11]2[c:12]([cH:13]1)[C:14]([CH3:15])([CH3:16])[O:17][C:18](=[O:19])[NH:20]2.OB(O)[c:7]1[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[cH:21]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]3[c:12]([cH:13]2)[C:14]([CH3:15])([CH3:16])[O:17][C:18](=[O:19])[NH:20]3)[cH:21]1
CC1(C)OC(=O)Nc2ccc(Br)cc21.COc1cccc(B(O)O)c1
COc1cccc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:5]:[c:4]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:2]:[c:3]
null
[]
null
null
null
null
6-(3-Methoxy-phenyl)-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one was prepared, according to the procedure of Example 4 from 6-bromo-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one and 3-methoxyphenyl boronic acid, as a yellow solid: mp 164–165° C.; 1H-NMR (DMSO-d6) δ 10.3 (s, 1H), 7.56 (m, 2H), 7.36 (t, 1H, J...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccccc1.c1ccc2c(c1)COCN2
c1ccccc1.c1ccc2c(c1)COCN2
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(Br)cc21.COc1cccc(B(O)O)c1>>COc1cccc(-c2ccc3c(c2)C(C)(C)OC(=O)N3)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c65c670bafc04607af088527d5e2523f
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1ccccc1Cl>>CC1(C)OC(=O)Nc2ccc(-c3ccccc3Cl)cc21
BrC1=CC2=C(NC(OC2(C)C)=O)C=C1.ClC1=C(C=CC=C1)B(O)O>>ClC1=C(C=CC=C1)C1=CC2=C(NC(OC2(C)C)=O)C=C1
Br[c:11]1[cH:10][cH:9][c:8]2[c:20]([cH:19]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.OB(O)[c:12]1[cH:13][cH:14][cH:15][cH:16][c:17]1[Cl:18]>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[Cl:18])[cH:19][c:20]21
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1ccccc1Cl
CC1(C)OC(=O)Nc2ccc(-c3ccccc3Cl)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](-[Cl;D1;H0:10]):[c:11]>>[Cl;D1;H0:10]-[c:9](:[c:11]):[c;H0;D3;+0:6](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:7]:[c:8]
null
[]
null
null
null
null
6-(2-Chloro-phenyl)-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one was prepared, according to the procedure of Example 4 from 6-bromo-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one and 2-chlorophenyl boronic acid, as a white solid: mp 181–182° C.; MS (ESI) m/z 288 ([M+H]+, 70%); Anal. Calc. For C16H14ClNO2: C, ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(Br)cc21.OB(O)c1ccccc1Cl>>CC1(C)OC(=O)Nc2ccc(-c3ccccc3Cl)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ae820404baa34a94b4d3ec0b616c8986
CC(O)(Cc1ccccc1)c1cc(-c2cccc(Cl)c2)ccc1N.O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl>>CC1(Cc2ccccc2)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
NC1=C(C=C(C=C1)C1=CC(=CC=C1)Cl)C(C)(O)CC1=CC=CC=C1.NC1=C(C=C(C=C1)C1=CC(=CC=C1)Cl)C(C)=O.C(C1=CC=CC=C1)[Mg]Br.ClC(Cl)(OC(OC(Cl)(Cl)Cl)=O)Cl>>C(C1=CC=CC=C1)C1(C2=C(NC(O1)=O)C=CC(=C2)C2=CC(=CC=C2)Cl)C
[CH3:1][C:2]([CH2:3][c:4]1[cH:5][cH:6][cH:7][cH:8][cH:9]1)([OH:10])[c:26]1[c:14]([NH2:13])[cH:15][cH:16][c:17](-[c:18]2[cH:19][cH:20][cH:21][c:22]([Cl:23])[cH:24]2)[cH:25]1.ClC(Cl)(Cl)O[C:11](OC(Cl)(Cl)Cl)=[O:12]>>[CH3:1][C:2]1([CH2:3][c:4]2[cH:5][cH:6][cH:7][cH:8][cH:9]2)[O:10][C:11](=[O:12])[NH:13][c:14]2[cH:15][cH:1...
CC(O)(Cc1ccccc1)c1cc(-c2cccc(Cl)c2)ccc1N.O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl
CC1(Cc2ccccc2)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
null
null
C1CCOC1
Protection
OtherReaction
2aea0be1056e79f2bca707804aa8e85c0a3e7237a1d4596f980bbb552d0f903a
5281b9a3f1004ab22b65d22fa67f63481ebe385cacff32b87d9504f5f5492462
O=C1Nc2ccc(-c3ccccc3)cc2C(Cc2ccccc2)O1
Cl-C(-Cl)(-Cl)-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-O-C(-Cl)(-Cl)-Cl.[C:3]-[C:4](-[C;D1;H3:5])(-[OH;D1;+0:6])-[c:7]:[c:8](-[NH2;D1;+0:9]):[c:10]>>[C:3]-[C:4]1(-[C;D1;H3:5])-[O;H0;D2;+0:6]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:9]-[c:8](:[c:10]):[c:7]-1
30
[{"value": 30.0, "product": "C(C1=CC=CC=C1)C1(C2=C(NC(O1)=O)C=CC(=C2)C2=CC(=CC=C2)Cl)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 1-(4-amino-3′-chloro-biphenyl-3-yl)-1-benzyl-ethanol (prepared from 1-(4-amino-3′-chloro-biphenyl-3-yl)-ethanone and benzylmagnesium bromide according to procedure described previously, 0.14 g, 0.42 mmol) and triphosgene (0.04 g, 0.14 mmol) in dry THF (10 mL) was stirred under a blanket of nitrogen for 10 ...
10.6084/m9.figshare.5104873.v1
null
Trichloro group.Trichloro group.Carbonic Ester.Tertiary alcohol.Primary amine
Carbamic ester
null
c1ccc2c(c1)COCN2
c1ccccc1.c1ccc2c(c1)COCN2.c1ccccc1
HCl
C1CCOC1
null
null
CC(O)(Cc1ccccc1)c1cc(-c2cccc(Cl)c2)ccc1N.O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl>C1CCOC1>CC1(Cc2ccccc2)OC(=O)Nc2ccc(-c3cccc(Cl)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1e7f65f8f38f4adfa5c342fff0841462
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(Br)cc(Br)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC1=CC(=CC(=C1)F)Br>>BrC=1C=C(C=C(C1)F)C1=CC2=C(NC(OC2(C)C)=O)C=C1
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:21]([cH:20]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][c:14]([F:15])[cH:16][c:17]([Br:18])[cH:19]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][c:14]([F:15])[cH:16][c:17]([Br:18])[cH:19]3)[cH:20][c:21]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(Br)cc(Br)c1
CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0fa2a30709dcd56081dfd73304ec3a2ee5346cb80b80e4b5dc426c319dd3d4bb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
null
[]
null
null
null
null
6-(3-Bromo-5-fluorophenyl)-4,4-dimethyl-1,4-dihydrobenzo[d][1,3]oxazin-2-one was prepared, from (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and 1,3-dibromo-5-fluorobenzene following the procedure of Example 5, as a white solid: mp 182–183° C.; 1H-NMR (DMSO-d6) δ 10.36 (s, 1H, D2O exchangeable), ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.Fc1cc(Br)cc(Br)c1>>CC1(C)OC(=O)Nc2ccc(-c3cc(F)cc(Br)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fe65bebe1e3a4f72a7a1f4060882e9df
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1ccc(Br)s1>>CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)s3)cc21
BrC1=CC=C(S1)C#N.CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C2=CC=C(S2)C#N)C
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:20]([cH:19]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][cH:14][c:15]([C:16]#[N:17])[s:18]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([C:16]#[N:17])[s:18]3)[cH:19][c:20]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1ccc(Br)s1
CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)s3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0b5bebfae8e49ed7172cda779db0d9a1ee34897b702e6169adb1825468a1d911
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3cccs3)cc2CO1
Br-[c;H0;D3;+0:1]1:[#16;a:2]:[c:3]:[c:4]:[c:5]:1.O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:10]:[c:9]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1]1:[#16;a:2]:[c:3]:[c:4]:[c:5]:1):[c:7]:[c:8]
null
[]
null
null
null
null
5-(4,4-Dimethyl-2-oxo-1,4-dihydro-2H-benzo[d][1,3]oxazin-6-yl)-thiophene-2-carbonitrile was prepared, according to the procedure of Example 5 using 5-bromo-2-thiophenecarbonitrile and (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid, as an off-white solid: mp 264–266° C.; 1H-NMR (DMSO-d6) δ 10.3 (s, ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccsc1
c1ccc2c(c1)COCN2.c1ccsc1
c1ccc2c(c1)COCN2.c1ccsc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1ccc(Br)s1>>CC1(C)OC(=O)Nc2ccc(-c3ccc(C#N)s3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fb8a7cb9b84a4ed1948475ce66754281
CC1(C)OC(=O)Nc2ccc(Br)cc21.Fc1ccc(Br)cc1Cl>>CC1(C)OC(=O)Nc2ccc(-c3ccc(F)c(Cl)c3)cc21
BrC1=CC2=C(NC(OC2(C)C)=O)C=C1.BrC1=CC(=C(C=C1)F)Cl>>ClC=1C=C(C=CC1F)C1=CC2=C(NC(OC2(C)C)=O)C=C1
Br[c:11]1[cH:10][cH:9][c:8]2[c:21]([cH:20]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][cH:14][c:15]([F:16])[c:17]([Cl:18])[cH:19]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([F:16])[c:17]([Cl:18])[cH:19]3)[cH:20][c:21]21
CC1(C)OC(=O)Nc2ccc(Br)cc21.Fc1ccc(Br)cc1Cl
CC1(C)OC(=O)Nc2ccc(-c3ccc(F)c(Cl)c3)cc21
null
null
null
C-C Coupling
Negishi
98598d81856d2c897d85eeb92f31247576a7bcf3cc7c3b939bc0c81fa93e6b1e
a7a4ce9a92e2f8a62d28956a69a5cc384426ab72416e87d68c6a3feb23c22d66
O=C1Nc2ccc(-c3ccccc3)cc2CO1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].Br-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:8]:[c:7]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:9]:[c:10]
null
[]
null
null
null
null
6-(3-Chloro-4-fluoro-phenyl)-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one was prepared, from 6-bromo-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one and 1-bromo-3-chloro-4-fluorobenzene according to Procedure A, as a white solid: mp 211–212° C.; 1H-NMR (DMSO-d6) δ 10.4 (s, 1H), 7.92 (dd, 1H, J=7.13, 2.19 Hz), ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide
null
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
c1ccc2c(c1)COCN2.c1ccccc1
Br-
null
null
null
CC1(C)OC(=O)Nc2ccc(Br)cc21.Fc1ccc(Br)cc1Cl>>CC1(C)OC(=O)Nc2ccc(-c3ccc(F)c(Cl)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d8a65d0330024d84bd2d3d89dfe8eeca
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cc(Br)co1>>CC1(C)OC(=O)Nc2ccc(-c3coc(C#N)c3)cc21
CC1(OC(NC2=C1C=C(C=C2)B(O)O)=O)C.BrC=1C=C(OC1)C#N>>CC1(C2=C(NC(O1)=O)C=CC(=C2)C=2C=C(OC2)C#N)C
OB(O)[c:11]1[cH:10][cH:9][c:8]2[c:20]([cH:19]1)[C:2]([CH3:1])([CH3:3])[O:4][C:5](=[O:6])[NH:7]2.Br[c:12]1[cH:13][o:14][c:15]([C:16]#[N:17])[cH:18]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][o:14][c:15]([C:16]#[N:17])[cH:18]3)[cH:19][c:20]21
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cc(Br)co1
CC1(C)OC(=O)Nc2ccc(-c3coc(C#N)c3)cc21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
4f7d7b24f806b5cd4e85a32312d9881a35e9e6beb03f90f98c00ef7f864a3ecf
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C1Nc2ccc(-c3ccoc3)cc2CO1
Br-[c;H0;D3;+0:1]1:[c:2]:[#8;a:3]:[c:4](-[C:5]#[N;D1;H0:6]):[c:7]:1.O-B(-O)-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]>>[N;D1;H0:6]#[C:5]-[c:4]1:[#8;a:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]):[c:7]:1
null
[]
null
null
null
null
4-(4,4-Dimethyl-2-oxo-1,4-dihydro-2H-benzo[d][1,3]oxazin-6-yl)-furan-2-carbonitrile was prepared from (1,4-dihydro-4,4-dimethyl-2-oxo-2H-3,1-benzoxazin-6-yl)boronic acid and 4-bromo-2-furancarbonitrile according to Procedure B. Off-white solid: mp 255–256° C. 1H-NMR (DMSO-d6) δ 10.32 (s, 1H, D2O exchangeable), 8.57 (s,...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)COCN2.c1ccoc1
c1ccc2c(c1)COCN2.c1ccoc1
c1ccc2c(c1)COCN2.c1ccoc1
HBr.B
null
null
null
CC1(C)OC(=O)Nc2ccc(B(O)O)cc21.N#Cc1cc(Br)co1>>CC1(C)OC(=O)Nc2ccc(-c3coc(C#N)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6d8f6eefee55419da012d50fe760f6de
CC1(C)OC(=O)Nc2ccc(-c3cccc(Br)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>>CC1(C)OC(=S)Nc2ccc(-c3cccc(Br)c3)cc21
BrC=1C=C(C=CC1)C1=CC2=C(NC(OC2(C)C)=O)C=C1.COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC>>BrC=1C=C(C=CC1)C=1C=CC2=C(C(OC(N2)=S)(C)C)C1
O=[C:5]1[O:4][C:2]([CH3:1])([CH3:3])[c:20]2[c:8]([cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([Br:17])[cH:18]3)[cH:19]2)[NH:7]1.COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:6])S2)cc1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[S:6])[NH:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][c:16]([Br:17])[cH:18]3)[cH:19][c:...
CC1(C)OC(=O)Nc2ccc(-c3cccc(Br)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
CC1(C)OC(=S)Nc2ccc(-c3cccc(Br)c3)cc21
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
97d5668e697b90041eba9dad68ad83f7a1cdfe0944b559f928d28ab2564e8d10
c331ef400a59f343eb23abd2f965cf1719390c2753d5de53af30054e75d29d94
S=C1Nc2ccc(-c3ccccc3)cc2CO1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.O=[C;H0;D3;+0:2](-[#7:3]-[c:4])-[#8:5]-[C:6]>>[C:6]-[#8:5]-[C;H0;D3;+0:2](=[S;H0;D1;+0:1])-[#7:3]-[c:4]
122.9
[{"value": 61.0, "product": "BrC=1C=C(C=CC1)C=1C=CC2=C(C(OC(N2)=S)(C)C)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 122.9, "product": "BrC=1C=C(C=CC1)C=1C=CC2=C(C(OC(N2)=S)(C)C)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
110
CELSIUS
null
null
A mixture of 6-(3-bromo-phenyl)-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one (3 g, 9.04 mmol) and Lawesson's Reagent (1.83 g, 4.51 mmol) in toluene (30 mL) was heated to 110° C. for 24 hours. The reaction was cooled, the toluene removed in vacuo and the residue purified via flash chromatography (silica gel, 20% e...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Ether.Monosulfide.Monosulfide
Ether.Thioamide
c1ccc2c(c1)COCN2.c1ccccc1.P1SPS1.c1ccccc1
c1ccc2c(c1)COCN2
c1ccc2c(c1)COCN2.c1ccccc1
Other
C1(=CC=CC=C1)C
110
null
CC1(C)OC(=O)Nc2ccc(-c3cccc(Br)c3)cc21.COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1>C1(=CC=CC=C1)C>CC1(C)OC(=S)Nc2ccc(-c3cccc(Br)c3)cc21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7712dc9388da484a8a072bcd7f76f278
O=c1c2c[nH]c3c(F)cccc3c-2nn1-c1ccc([N+](=O)[O-])cc1>>Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1
C(C)(=O)OCC.O.O.[Sn](Cl)Cl.[N+](=O)([O-])C1=CC=C(C=C1)N1N=C2C(=CNC=3C(=CC=CC23)F)C1=O.[N+](=O)([O-])C1=CC=C(C=C1)N1N=C2C(=CNC=3C(=CC=CC23)F)C1=O.C([O-])(O)=O.[Na+]>>NC1=CC=C(C=C1)N1N=C2C(=CNC=3C(=CC=CC23)F)C1=O
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][c:5](-[n:6]2[n:7][c:8]3[c:9]4[cH:10][cH:11][cH:12][c:13]([F:14])[c:15]4[nH:16][cH:17][c:18]-3[c:19]2=[O:20])[cH:21][cH:22]1>>[NH2:1][c:2]1[cH:3][cH:4][c:5](-[n:6]2[n:7][c:8]3[c:9]4[cH:10][cH:11][cH:12][c:13]([F:14])[c:15]4[nH:16][cH:17][c:18]-3[c:19]2=[O:20])[cH:21][cH:22]1
O=c1c2c[nH]c3c(F)cccc3c-2nn1-c1ccc([N+](=O)[O-])cc1
Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1
null
null
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=c1c2c[nH]c3ccccc3c-2nn1-c1ccccc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
104.7
[{"value": 99.0, "product": "NC1=CC=C(C=C1)N1N=C2C(=CNC=3C(=CC=CC23)F)C1=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 104.7, "product": "NC1=CC=C(C=C1)N1N=C2C(=CNC=3C(=CC=CC23)F)C1=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
Tin (II) chloride dihydrate (12.5 g, 0.055 mol) was added in one portion to a stirred solution of 2-(4-nitro-phenyl)-6-fluoro-2,5-dihydro-pyrazolo[4,3-c]quinolin-3-one (intermediate 1) (3.59 g, 0.011 mol) in ethyl alcohol (110 ml) at room temperature. The mixture was then heated to 80° C. for 8 h, cooled to room temper...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccc2c(c1)ncc1c[nH]nc12
Other
C(C)O
80
null
O=c1c2c[nH]c3c(F)cccc3c-2nn1-c1ccc([N+](=O)[O-])cc1>C(C)O>Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f5204a39d4c54ba09d8bf60f425a3b07
CCC(C)C(=O)Cl.Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1>>CCC(C)C(=O)Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1
CC(C(=O)Cl)CC.NC1=CC=C(C=C1)N1N=C2C(=CNC=3C(=CC=CC23)F)C1=O.NC1=CC=C(C=C1)N1N=C2C(=CNC=3C(=CC=CC23)F)C1=O.C(C)N(CC)CC>>FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C3=CC=C(C=C3)NC(C(CC)C)=O)=O
Cl[C:5]([CH:3]([CH2:2][CH3:1])[CH3:4])=[O:6].[NH2:7][c:8]1[cH:9][cH:10][c:11](-[n:12]2[n:13][c:14]3[c:15]4[cH:16][cH:17][cH:18][c:19]([F:20])[c:21]4[nH:22][cH:23][c:24]-3[c:25]2=[O:26])[cH:27][cH:28]1>>[CH3:1][CH2:2][CH:3]([CH3:4])[C:5](=[O:6])[NH:7][c:8]1[cH:9][cH:10][c:11](-[n:12]2[n:13][c:14]3[c:15]4[cH:16][cH:17][c...
CCC(C)C(=O)Cl.Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1
CCC(C)C(=O)Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1
null
CN(C1=CC=NC=C1)C
ClCCl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
O=c1c2c[nH]c3ccccc3c-2nn1-c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C;D1;H3:5].[NH2;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[C:4]-[C:3](-[C;D1;H3:5])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]
26.4
[{"value": 26.0, "product": "FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C3=CC=C(C=C3)NC(C(CC)C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 26.4, "product": "FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C3=CC=C(C=C3)NC(C(CC)C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
(±)-2-Methylbutyryl chloride (13.6 μl, 0.11 mmol) was added dropwise over 30 sec to a stirred solution of 2-(4-amino-phenyl)-6-fluoro-2,5-dihydro-pyrazolo[4,3-c]quinolin-3-one (Intermediate 2) (30 mg, 0.10 mmol), triethylamine (14 μl, 0.11 mmol) and 4-dimethylaminopyridine (2.4 mg, 0.02 mmol) in dichloromethane (1 ml) ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccc2c(c1)ncc1c[nH]nc12
HCl
CN(C1=CC=NC=C1)C.ClCCl
null
16
CCC(C)C(=O)Cl.Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1>CN(C1=CC=NC=C1)C.ClCCl>CCC(C)C(=O)Nc1ccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-866ba5d8f9af45bb90727795f570a17b
CCOC(=O)c1cnc2c(F)cccc2c1Cl.NNc1cccc(C(=O)O)c1>>O=C(O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
Cl.N(N)C=1C=C(C(=O)O)C=CC1.C(C)OC(=O)C=1C=NC2=C(C=CC=C2C1Cl)F.[OH-].[Li+]>>FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)O)C=CC3)=O
CCO[C:22]([c:21]1[c:11](Cl)[c:12]2[cH:13][cH:14][cH:15][c:16]([F:17])[c:18]2[n:19][cH:20]1)=[O:23].[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][cH:7][c:8]([NH:9][NH2:10])[cH:24]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][cH:7][c:8](-[n:9]2[n:10][c:11]3[c:12]4[cH:13][cH:14][cH:15][c:16]([F:17])[c:18]4[nH:19][cH:20][c:21]-3[c:22]2...
CCOC(=O)c1cnc2c(F)cccc2c1Cl.NNc1cccc(C(=O)O)c1
O=C(O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
null
null
C(CCC)O.O1CCCC1.O
Aromatic Heterocycle Formation
OtherReaction
ee439f0d33eddb680aeae010a39ecb3e522826f644f963c6ba8a62694a2e2b1e
20cc0446e4e8da9890d540018d45591431260c9e839f50bab7497c80b683dbef
O=c1c2c[nH]c3ccccc3c-2nn1-c1ccccc1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:3]1:[c:4]:[n;H0;D2;+0:5]:[c:6](:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:10]:1-Cl.[NH2;D1;+0:11]-[NH;D2;+0:12]-[c;H0;D3;+0:13](:[c:14]:[c:15]-[C:16](=[O;D1;H0:17])-[O;D1;H1:18]):[c:19]:[c:20]>>[O;D1;H0:17]=[C:16](-[O;D1;H1:18])-[c:15]:[c:14]:[c;H0;D3;+0:13](-[n;H0;D3;+0:12]1:[n;H0...
65.2
[{"value": 63.0, "product": "FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)O)C=CC3)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 65.2, "product": "FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)O)C=CC3)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
3-Hydrazinobenzoic acid (1.91 g, 0.013 mol) was added in one portion to a stirred solution of 4-chloro-8-fluoro-quinoline-3-carboxylic acid ethyl ester (2.93 g, 0.011 mol) in n-butanol (60 ml) at room temperature. The solution was heated to reflux for 16 h, cooled to room temperature and the resulting yellow solid filt...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Aromatic halide.Ester
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1c[nH]nc12
c1ccccc1.c1ccc2c(c1)ncc1c[nH]nc12
HCl
C(CCC)O.O1CCCC1.O
null
16
CCOC(=O)c1cnc2c(F)cccc2c1Cl.NNc1cccc(C(=O)O)c1>C(CCC)O.O1CCCC1.O>O=C(O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b99d872116fe4931a25f64e611601e06
O=C(Cl)C(=O)Cl.O=C(O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1>>O=C(Cl)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
CN(C=O)C.C(C(=O)Cl)(=O)Cl.FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)O)C=CC3)=O.FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)O)C=CC3)=O>>FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)Cl)C=CC3)=O
O=C(Cl)C(=O)[Cl:3].O[C:2](=[O:1])[c:4]1[cH:5][cH:6][cH:7][c:8](-[n:9]2[n:10][c:11]3[c:12]4[cH:13][cH:14][cH:15][c:16]([F:17])[c:18]4[nH:19][cH:20][c:21]-3[c:22]2=[O:23])[cH:24]1>>[O:1]=[C:2]([Cl:3])[c:4]1[cH:5][cH:6][cH:7][c:8](-[n:9]2[n:10][c:11]3[c:12]4[cH:13][cH:14][cH:15][c:16]([F:17])[c:18]4[nH:19][cH:20][c:21]-3[...
O=C(Cl)C(=O)Cl.O=C(O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
O=C(Cl)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
null
null
ClCCl
Functional Group Interconversion
Alcohol to chloride_Other
013cec2edeb273a7a148f349d36a52d99ff4e7bcf8eed78085df830088e387ac
aedb1f68dc5b7eb0583043e1125b741382b17974140a2f46554f0110e2ddc884
O=c1c2c[nH]c3ccccc3c-2nn1-c1ccccc1
Cl-C(=O)-C(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]>>[Cl;H0;D1;+0:1]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
96
[{"value": 96.0, "product": "FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)Cl)C=CC3)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.9, "product": "FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)Cl)C=CC3)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
null
null
Oxalyl chloride (20 ml, 0.2 mol) was added dropwise over 2 min to a stirred solution of 3-(6-fluoro-3-oxo-3,5-dihydro-pyrazolo[4,3-c]quinolin-2-yl)-benzoic acid (intermediate 3) (2.0 g, 6.1 mmol) in dichloromethane (10 ml) at room temperature. N,N-Dimethylformamide (50 μl) was then added and the resulting mixture heate...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Carboxylic acid
Acyl halide
null
null
c1ccccc1.c1ccc2c(c1)ncc1c[nH]nc12
HCl
ClCCl
50
null
O=C(Cl)C(=O)Cl.O=C(O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1>ClCCl>O=C(Cl)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-17c5c40e4c584119be22329d4d1bff41
COCCCN.O=C(Cl)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1>>COCCCNC(=O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
C(C)N(CC)CC.COCCCN.FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)Cl)C=CC3)=O.FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)Cl)C=CC3)=O.Cl>>FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)NCCCOC)C=CC3)=O
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][NH2:6].Cl[C:7](=[O:8])[c:9]1[cH:10][cH:11][cH:12][c:13](-[n:14]2[n:15][c:16]3[c:17]4[cH:18][cH:19][cH:20][c:21]([F:22])[c:23]4[nH:24][cH:25][c:26]-3[c:27]2=[O:28])[cH:29]1>>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][NH:6][C:7](=[O:8])[c:9]1[cH:10][cH:11][cH:12][c:13](-[n:14]2[n:15][c:16]3[c:17]...
COCCCN.O=C(Cl)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
COCCCNC(=O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
null
null
O1CCCC1
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
O=c1c2c[nH]c3ccccc3c-2nn1-c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
69
[{"value": 69.0, "product": "FC1=CC=CC=2C=3C(=CNC12)C(N(N3)C=3C=C(C(=O)NCCCOC)C=CC3)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
3-Methoxypropylamine (0.026 g, 0.29 mmol) was added to a stirred solution of 3-(6-fluoro-3-oxo-3,5-dihydro-pyrazolo[4,3-c]quinolin-2-yl)-benzoyl chloride (intermediate 4) (26 mg 0.29 mmol) in tetrahydrofuran (2 ml) and the mixture stirred at room temperature for 15 min. Triethylamine (0.2 ml, 1.4 mmol) was then added a...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccc2c(c1)ncc1c[nH]nc12
HCl
O1CCCC1
null
0.25
COCCCN.O=C(Cl)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1>O1CCCC1>COCCCNC(=O)c1cccc(-n2nc3c4cccc(F)c4[nH]cc-3c2=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9c5e52f4a35d4393b82cadb4af74d145
CCOC(=O)c1ccccc1N.COC(=O)CC(=O)C1CC1>>CCOC(=O)c1c(C2CC2)[nH]c2ccccc2c1=O
COC(CC(=O)C1CC1)=O.C(C)OC(C1=C(C=CC=C1)N)=O.C1(=CC=CC=C1)C>>C(C)OC(=O)C1=C(NC2=CC=CC=C2C1=O)C1CC1
[CH3:1][CH2:2][O:3][C:18]([c:17]1[c:12]([NH2:11])[cH:13][cH:14][cH:15][cH:16]1)=[O:19].CO[C:4](=[O:5])[CH2:6][C:7](=O)[CH:8]1[CH2:9][CH2:10]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH:8]2[CH2:9][CH2:10]2)[nH:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[c:18]1=[O:19]
CCOC(=O)c1ccccc1N.COC(=O)CC(=O)C1CC1
CCOC(=O)c1c(C2CC2)[nH]c2ccccc2c1=O
null
C1(=CC=C(C=C1)S(=O)(=O)O)C
null
Aromatic Heterocycle Formation
OtherReaction
491bd2fdcb2b219c36e07712d3416b2b20d234f8420994329b56ea19314c754b
1f7cfbf178b989a5dc61b8bb4fcd61ce54e19d0cd6c69f55ae836eb22030509b
O=c1cc(C2CC2)[nH]c2ccccc12
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH2;D2;+0:3]-[C;H0;D3;+0:4](=O)-[C:5]1-[C:6]-[C:7]-1.[C;D1;H3:8]-[C:9]-[O;H0;D2;+0:10]-[C;H0;D3;+0:11](=[O;D1;H0:12])-[c:13](:[c:14]):[c:15](-[NH2;D1;+0:16]):[c:17]>>[C;D1;H3:8]-[C:9]-[O;H0;D2;+0:10]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:3]1:[c;H0;D3;+0:11](=[O;D1;H0:12]):[c:13](:[c...
53
[{"value": 53.0, "product": "C(C)OC(=O)C1=C(NC2=CC=CC=C2C1=O)C1CC1", "details": "PERCENTYIELD", "is_desired": false}]
120
CELSIUS
2
HOUR
A solution of 3-cyclopropyl-3-oxo-propionic acid methyl ester (6.2 g, 0.038 mols), 2-amino benzoic acid ethyl ester (4.95 g, 0.03 mols) and p-toluene sulfonic acid (0.04 g, 0.2 mmols) in toluene (25 ml) was heated at 125° C. for 2 h; 15 ml of solvent was then distilled. To the residual orange solution was added sodium ...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Ester.Primary amine
Ester
c1ccccc1
c1cnc2ccccc2c1
C1CC1.c1cnc2ccccc2c1
HO-
C1(=CC=C(C=C1)S(=O)(=O)O)C
120
2
CCOC(=O)c1ccccc1N.COC(=O)CC(=O)C1CC1>C1(=CC=C(C=C1)S(=O)(=O)O)C>CCOC(=O)c1c(C2CC2)[nH]c2ccccc2c1=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4872319f5f1945ae911cbcc86e7b9e1a
CCOC(=O)c1c(C2CC2)[nH]c2ccccc2c1=O.O=P(Cl)(Cl)Cl>>CCOC(=O)c1c(C2CC2)nc2ccccc2c1Cl
P(=O)(Cl)(Cl)Cl.C(C)OC(=O)C1=C(NC2=CC=CC=C2C1=O)C1CC1.C([O-])(O)=O.[Na+]>>C(C)OC(=O)C=1C(=NC2=CC=CC=C2C1Cl)C1CC1
O=[c:18]1[c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:7]([CH:8]2[CH2:9][CH2:10]2)[nH:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]21.O=P(Cl)(Cl)[Cl:19]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[c:7]([CH:8]2[CH2:9][CH2:10]2)[n:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[c:18]1[Cl:19]
CCOC(=O)c1c(C2CC2)[nH]c2ccccc2c1=O.O=P(Cl)(Cl)Cl
CCOC(=O)c1c(C2CC2)nc2ccccc2c1Cl
null
null
C(C)#N
Functional Group Interconversion
OtherReaction
608f63cb1f4eb5f8ff4f6128056e651e12d8905ddec242decf5bdb71da52a2d7
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc2nc(C3CC3)ccc2c1
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].O=[c;H0;D3;+0:2]1:[c:3](:[c:4]):[c:5](:[c:6]):[nH;D2;+0:7]:[c:8](-[C:9]):[c:10]:1-[C:11](=[O;D1;H0:12])-[#8:13]-[C:14]>>[C:14]-[#8:13]-[C:11](=[O;D1;H0:12])-[c:10]1:[c:8](-[C:9]):[n;H0;D2;+0:7]:[c:5](:[c:6]):[c:3](:[c:4]):[c;H0;D3;+0:2]:1-[Cl;H0;D1;+0:1]
106
[{"value": 106.0, "product": "C(C)OC(=O)C=1C(=NC2=CC=CC=C2C1Cl)C1CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 10.2, "product": "C(C)OC(=O)C=1C(=NC2=CC=CC=C2C1Cl)C1CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
75
CELSIUS
null
null
Phosphorus oxychloride (0.77 ml, 0.082 mols) was added in one portion to a suspension of 2-cyclopropyl-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid ethyl ester (1.0 g, 0.041 mols) in acetonitrile and the mixture was heated at 75° C. for 90 minutes (becomes a clear solution above 65° C.). The resulting light brown solu...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1cnc2ccccc2c1
c1ccc2ncccc2c1
C1CC1.c1ccc2ncccc2c1
HCl
C(C)#N
75
null
CCOC(=O)c1c(C2CC2)[nH]c2ccccc2c1=O.O=P(Cl)(Cl)Cl>C(C)#N>CCOC(=O)c1c(C2CC2)nc2ccccc2c1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-924acceae61043aa9030a239df61f749
CCOC(=O)c1c(C2CC2)nc2ccccc2c1Cl.NNc1ccc(C(=O)O)cc1>>O=C(O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
C(C)OC(=O)C=1C(=NC2=CC=CC=C2C1Cl)C1CC1.N(N)C1=CC=C(C(=O)O)C=C1.NN>>C1(CC1)C=1NC=2C=CC=CC2C=2C1C(N(N2)C2=CC=C(C(=O)O)C=C2)=O
CCO[C:23]([c:22]1[c:10](Cl)[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[n:17][c:18]1[CH:19]1[CH2:20][CH2:21]1)=[O:24].[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]([NH:8][NH2:9])[cH:25][cH:26]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7](-[n:8]2[n:9][c:10]3[c:11]4[cH:12][cH:13][cH:14][cH:15][c:16]4[nH:17][c:18]([CH:19]4[CH2...
CCOC(=O)c1c(C2CC2)nc2ccccc2c1Cl.NNc1ccc(C(=O)O)cc1
O=C(O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
null
null
Cl.CCCCCCC.C(C)O
Aromatic Heterocycle Formation
OtherReaction
ee439f0d33eddb680aeae010a39ecb3e522826f644f963c6ba8a62694a2e2b1e
20cc0446e4e8da9890d540018d45591431260c9e839f50bab7497c80b683dbef
O=c1c2c(C3CC3)[nH]c3ccccc3c-2nn1-c1ccccc1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:3]1:[c:4](-[C:5]):[n;H0;D2;+0:6]:[c:7](:[c:8]):[c:9](:[c:10]):[c;H0;D3;+0:11]:1-Cl.[NH2;D1;+0:12]-[NH;D2;+0:13]-[c;H0;D3;+0:14](:[c:15]:[c:16]):[c:17]:[c:18]>>[C:5]-[c:4]1:[nH;D2;+0:6]:[c:7](:[c:8]):[c:9](:[c:10]):[c;H0;D3;+0:11]2:[n;H0;D2;+0:12]:[n;H0;D3;+0:13](-[c;H0;D3;...
80.2
[{"value": 80.0, "product": "C1(CC1)C=1NC=2C=CC=CC2C=2C1C(N(N2)C2=CC=C(C(=O)O)C=C2)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 80.2, "product": "C1(CC1)C=1NC=2C=CC=CC2C=2C1C(N(N2)C2=CC=C(C(=O)O)C=C2)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-chloro-2-cyclopropyl-quinoline-3-carboxylic acid ethyl ester (1.15 g, 0.0041 mols) and 4-hydrazino-benzoic acid (1.0 g, 0.0068 mols) were stirred in ethanol (30 ml) at reflux for 16 h. The bright yellow suspension was diluted with heptane, filtered, washed with cold t-butylmethyl ether and left to dry under suction t...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Aromatic halide.Ester
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1c[nH]nc12
c1ccccc1.c1ccc2c(c1)ncc1c[nH]nc12.C1CC1
HCl
Cl.CCCCCCC.C(C)O
null
null
CCOC(=O)c1c(C2CC2)nc2ccccc2c1Cl.NNc1ccc(C(=O)O)cc1>Cl.CCCCCCC.C(C)O>O=C(O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c8319f031c8746a7bda69ce0ffb04f8a
O=C(Cl)C(=O)Cl.O=C(O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1>>O=C(Cl)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
C1(CC1)C=1NC=2C=CC=CC2C=2C1C(N(N2)C2=CC=C(C(=O)O)C=C2)=O.C(C(=O)Cl)(=O)Cl.CN(C=O)C>>C1(CC1)C=1NC=2C=CC=CC2C=2C1C(N(N2)C2=CC=C(C(=O)Cl)C=C2)=O
O=C(Cl)C(=O)[Cl:3].O[C:2](=[O:1])[c:4]1[cH:5][cH:6][c:7](-[n:8]2[n:9][c:10]3[c:11]4[cH:12][cH:13][cH:14][cH:15][c:16]4[nH:17][c:18]([CH:19]4[CH2:20][CH2:21]4)[c:22]-3[c:23]2=[O:24])[cH:25][cH:26]1>>[O:1]=[C:2]([Cl:3])[c:4]1[cH:5][cH:6][c:7](-[n:8]2[n:9][c:10]3[c:11]4[cH:12][cH:13][cH:14][cH:15][c:16]4[nH:17][c:18]([CH:...
O=C(Cl)C(=O)Cl.O=C(O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
O=C(Cl)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
null
null
ClCCl
Functional Group Interconversion
Alcohol to chloride_Other
013cec2edeb273a7a148f349d36a52d99ff4e7bcf8eed78085df830088e387ac
aedb1f68dc5b7eb0583043e1125b741382b17974140a2f46554f0110e2ddc884
O=c1c2c(C3CC3)[nH]c3ccccc3c-2nn1-c1ccccc1
Cl-C(=O)-C(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]>>[Cl;H0;D1;+0:1]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
null
[]
45
CELSIUS
8
HOUR
To a suspension of finely ground 4-(4-cyclopropyl-3-oxo-3,5-dihydro-pyrazolo[4,3-c]quinolin-2-yl)-benzoic acid (0.19 g. 0.55 mmol) in dichloromethane (4 ml) was added oxalyl chloride (1.6 ml, 0.01 mol) followed by a drop of dimethyl formamide. The mixture was stirred under nitrogen at 45° C. for 8 h. The solvent was re...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Carboxylic acid
Acyl halide
null
null
c1ccccc1.c1ccc2c(c1)ncc1c[nH]nc12.C1CC1
HCl
ClCCl
45
8
O=C(Cl)C(=O)Cl.O=C(O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1>ClCCl>O=C(Cl)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e5ce23572c0a4884939891bce2bc781d
CN(C)CCCN.O=C(Cl)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1>>CN(C)CCCNC(=O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
C1(CC1)C=1NC=2C=CC=CC2C=2C1C(N(N2)C2=CC=C(C(=O)Cl)C=C2)=O.CN(CCCN)C>>CN(CCCNC(C1=CC=C(C=C1)N1N=C2C(=C(NC=3C=CC=CC23)C2CC2)C1=O)=O)C
[CH3:1][N:2]([CH3:3])[CH2:4][CH2:5][CH2:6][NH2:7].Cl[C:8](=[O:9])[c:10]1[cH:11][cH:12][c:13](-[n:14]2[n:15][c:16]3[c:17]4[cH:18][cH:19][cH:20][cH:21][c:22]4[nH:23][c:24]([CH:25]4[CH2:26][CH2:27]4)[c:28]-3[c:29]2=[O:30])[cH:31][cH:32]1>>[CH3:1][N:2]([CH3:3])[CH2:4][CH2:5][CH2:6][NH:7][C:8](=[O:9])[c:10]1[cH:11][cH:12][c...
CN(C)CCCN.O=C(Cl)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
CN(C)CCCNC(=O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1
null
null
O1CCCC1
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
O=c1c2c(C3CC3)[nH]c3ccccc3c-2nn1-c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
47.4
[{"value": 47.0, "product": "CN(CCCNC(C1=CC=C(C=C1)N1N=C2C(=C(NC=3C=CC=CC23)C2CC2)C1=O)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 47.4, "product": "CN(CCCNC(C1=CC=C(C=C1)N1N=C2C(=C(NC=3C=CC=CC23)C2CC2)C1=O)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a partial solution of 4-(4-cyclopropyl-3-oxo-3,5-dihydro-pyrazolo[4,3-c]quinolin-2-yl)-benzoyl chloride (0.1 g, 0.28 mmol) in tetrahydrofurane (6 ml) under nitrogen was added a solution of 3-dimethylamino-propyl amine (0.03 g, 0.3 mmol) in tetrahydrofurane (3 ml). The mixture was stirred at RT for 3 h. The solvent w...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccc2c(c1)ncc1c[nH]nc12.C1CC1
HCl
O1CCCC1
null
3
CN(C)CCCN.O=C(Cl)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1>O1CCCC1>CN(C)CCCNC(=O)c1ccc(-n2nc3c4ccccc4[nH]c(C4CC4)c-3c2=O)cc1