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-c31cb9b44c404c10ba3aa533aa079e2b
ord-fac4a83c352644bd84e41f5061162643
C=O.CNC(CCc1ccc(OC)cc1)c1cccc(OC(=O)N(C)C)c1>>COc1ccc(CCC(c2cccc(OC(=O)N(C)C)c2)N(C)C)cc1
C=O.Cl.CN(C(OC1=CC(=CC=C1)C(CCC1=CC=C(C=C1)OC)NC)=O)C.[OH-].[Na+]>>CN(C(OC1=CC(=CC=C1)C(CCC1=CC=C(C=C1)OC)N(C)C)=O)C
O=[CH2:23].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][CH:9]([c:10]2[cH:11][cH:12][cH:13][c:14]([O:15][C:16](=[O:17])[N:18]([CH3:19])[CH3:20])[cH:21]2)[NH:22][CH3:24])[cH:25][cH:26]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][CH:9]([c:10]2[cH:11][cH:12][cH:13][c:14]([O:15][C:16](=[O:17])[N:18]([CH3:19])...
C=O.CNC(CCc1ccc(OC)cc1)c1cccc(OC(=O)N(C)C)c1
COc1ccc(CCC(c2cccc(OC(=O)N(C)C)c2)N(C)C)cc1
null
null
C(=O)O
Heteroatom Alkylation and Arylation
Eschweiler-Clarke Secondary Amine Methylation
deb0f39510ff32c3bd75ceaf7ece4070b1f686ff120d798ccd640765025dab3c
e1fdef8fde1c506d7c9deb8fd5e6f322eceea2abce3167abcf412a1fa4fd5443
c1ccc(CCCc2ccccc2)cc1
O=[CH2;D1;+0:1].[C:2]-[C:3](-[c:4])-[NH;D2;+0:5]-[C;D1;H3:6]>>[C:2]-[C:3](-[c:4])-[N;H0;D3;+0:5](-[C;D1;H3:6])-[CH3;D1;+0:1]
null
[]
90
CELSIUS
2
HOUR
Formic acid (10 ml) and 35% aqueous formaldehyde solution (10 ml) were added to 3-[3-(4-methoxyphenyl)-1-methylaminopropyl]phenyl dimethylcarbamate (500 mg, 1.4 mmol) obtained from Example 2 and the mixture was stirred at 90° C. for 2 hours. After cooling the reaction mixture to room temperature the mixture was neutral...
10.6084/m9.figshare.5104873.v1
null
Formaldehyde.Secondary amine
Tertiary amine
null
null
c1ccccc1.c1ccccc1
Other
C(=O)O
90
2
C=O.CNC(CCc1ccc(OC)cc1)c1cccc(OC(=O)N(C)C)c1>C(=O)O>COc1ccc(CCC(c2cccc(OC(=O)N(C)C)c2)N(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-0219005098e64f6d8b20ac6a432dba0e
CN.O=C(O)CC(=O)O.O=Cc1cccc(O)c1>>CNC(CC(=O)O)c1cccc(O)c1
OC=1C=C(C=O)C=CC1.C(CC(=O)O)(=O)O.C(C)(=O)O.CN>>OC=1C=C(C=CC1)C(CC(=O)O)NC
[CH3:1][NH2:2].O=C(O)[CH2:4][C:5](=[O:6])[OH:7].O=[CH:3][c:8]1[cH:9][cH:10][cH:11][c:12]([OH:13])[cH:14]1>>[CH3:1][NH:2][CH:3]([CH2:4][C:5](=[O:6])[OH:7])[c:8]1[cH:9][cH:10][cH:11][c:12]([OH:13])[cH:14]1
CN.O=C(O)CC(=O)O.O=Cc1cccc(O)c1
CNC(CC(=O)O)c1cccc(O)c1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
029574ef26de21f885bdd45bc4c594df31907abcec9280dfb6bae6d8c823e790
b3ae5256a03516152477e54cb65b2c8ce8e6de1b7a097a5a730c0f14a2ab31ca
c1ccccc1
O-C(=O)-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[O;D1;H1:4].O=[CH;D2;+0:5]-[c:6](:[c:7]):[c:8].[C;D1;H3:9]-[NH2;D1;+0:10]>>[C;D1;H3:9]-[NH;D2;+0:10]-[CH;D3;+0:5](-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[O;D1;H1:4])-[c:6](:[c:7]):[c:8]
58.8
[{"value": 58.8, "product": "OC=1C=C(C=CC1)C(CC(=O)O)NC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
3-Hydroxybenzaldehyde (25.7 g, 210 mmol) was dissolved in ethanol (70 ml), and malonic acid (25.7 g) and the acetic acid salt of methylamine (38.6 g) were added to the solution. The resulting mixture was heated under reflux for 3 hours. Crystals which precipitated in the reaction mixture were collected by filtration to...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Carboxylic acid.Primary amine
Secondary amine
null
null
c1ccccc1
HO-
C(C)O
null
null
CN.O=C(O)CC(=O)O.O=Cc1cccc(O)c1>C(C)O>CNC(CC(=O)O)c1cccc(O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8c444d6cd1494f348b8fe8d56c164586
CCO.CNC(CC(=O)O)c1cccc(O)c1>>CCOC(=O)CC(NC)c1cccc(O)c1
OC=1C=C(C=CC1)C(CC(=O)O)NC.C(C)O.S(O)(O)(=O)=O.C(O)([O-])=O.[Na+]>>OC=1C=C(C=CC1)C(CC(=O)OCC)NC
[CH3:1][CH2:2][OH:3].O[C:4](=[O:5])[CH2:6][CH:7]([NH:8][CH3:9])[c:10]1[cH:11][cH:12][cH:13][c:14]([OH:15])[cH:16]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]([NH:8][CH3:9])[c:10]1[cH:11][cH:12][cH:13][c:14]([OH:15])[cH:16]1
CCO.CNC(CC(=O)O)c1cccc(O)c1
CCOC(=O)CC(NC)c1cccc(O)c1
null
null
null
Protection
Esterification of Carboxylic Acids
070670f68a20c1021da94fabee54def4688122fb721af5f52cd5a03630845d0e
0d8a72b7375d91aa7263e766e03a3cb7c4fa91e27abcd590409ff03b98eed690
c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C;D1;H3:5]-[C:6]-[OH;D1;+0:7]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[O;H0;D2;+0:7]-[C:6]-[C;D1;H3:5]
null
[]
null
null
null
null
3-(3-Hydroxyphenyl)-3-methylaminopropionic acid (24.1 g) obtained from Example 7a was dissolved in ethanol (200 ml), and concentrated sulfuric acid (10 ml) was added dropwise to the solution. The resulting mixture was heated under reflux for 8 hours. The reaction mixture was neutralized with saturated aqueous sodium hy...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary alcohol
Ester
null
null
c1ccccc1
HO-
null
null
null
CCO.CNC(CC(=O)O)c1cccc(O)c1>>CCOC(=O)CC(NC)c1cccc(O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d175929ad14c40eebb87c51e8c9d33b0
BrCc1ccccc1.CCOC(=O)CC(c1ccc(O)cc1)N(C)C(=O)OC(C)(C)C>>CCOC(=O)CC(c1ccc(OCc2ccccc2)cc1)N(C)C(=O)OC(C)(C)C
C(C1=CC=CC=C1)Br.C(C)(C)(C)OC(=O)N(C)C(CC(=O)OCC)C1=CC=C(C=C1)O.C([O-])([O-])=O.[K+].[K+]>>C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CC(=O)OCC)N(C)C(=O)OC(C)(C)C
Br[CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1.[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]([c:8]1[cH:9][cH:10][c:11]([OH:12])[cH:20][cH:21]1)[N:22]([CH3:23])[C:24](=[O:25])[O:26][C:27]([CH3:28])([CH3:29])[CH3:30]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]([c:8]1[cH:9][cH:10][c:11]([O:12][CH2:13][c:14]2[cH:...
BrCc1ccccc1.CCOC(=O)CC(c1ccc(O)cc1)N(C)C(=O)OC(C)(C)C
CCOC(=O)CC(c1ccc(OCc2ccccc2)cc1)N(C)C(=O)OC(C)(C)C
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccc(COc2ccccc2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[c:7]:[c:6](-[O;H0;D2;+0:5]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]):[c:8]
84.2
[{"value": 84.2, "product": "C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CC(=O)OCC)N(C)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
N,N-Dimethylformamide and benzyl bromide (2.3 ml, 19 mmol) were added sequentially to ethyl 3-[N-(t-butoxy carbonyl)-N-methylamino]-3-(4-hydroxyphenyl)propionate (5.10 g, 16 mmol) obtained from Example 16a and potassium carbonate (3.27 g, 24 mmol) and the mixture was stirred at room temperature for 4 hours. The reactio...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1.c1ccccc1
HBr
CN(C=O)C
null
4
BrCc1ccccc1.CCOC(=O)CC(c1ccc(O)cc1)N(C)C(=O)OC(C)(C)C>CN(C=O)C>CCOC(=O)CC(c1ccc(OCc2ccccc2)cc1)N(C)C(=O)OC(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-05b22ece25a14d5396cd84f1b34ecfac
CCOC(=O)CC(c1ccc(OCc2ccccc2)cc1)N(C)C(=O)OC(C)(C)C>>CN(C(=O)OC(C)(C)C)C(CCO)c1ccc(OCc2ccccc2)cc1
S(=O)(=O)([O-])[O-].[Mg+2].[OH-].[Na+].C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CC(=O)OCC)N(C)C(=O)OC(C)(C)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CCO)N(C(OC(C)(C)C)=O)C
CCO[C:12]([CH2:11][CH:10]([N:2]([CH3:1])[C:3](=[O:4])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9])[c:14]1[cH:15][cH:16][c:17]([O:18][CH2:19][c:20]2[cH:21][cH:22][cH:23][cH:24][cH:25]2)[cH:26][cH:27]1)=[O:13]>>[CH3:1][N:2]([C:3](=[O:4])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9])[CH:10]([CH2:11][CH2:12][OH:13])[c:14]1[cH:15][cH:16][c:17...
CCOC(=O)CC(c1ccc(OCc2ccccc2)cc1)N(C)C(=O)OC(C)(C)C
CN(C(=O)OC(C)(C)C)C(CCO)c1ccc(OCc2ccccc2)cc1
null
null
O1CCCC1.O
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(COc2ccccc2)cc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]-[C:4]>>[C:4]-[C:3]-[CH2;D2;+0:1]-[OH;D1;+0:2]
99
[{"value": 99.0, "product": "C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CCO)N(C(OC(C)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
Tetrahydrofuran (100 ml) was added to lithium aluminum hydride (1.02 g, 27 mmol) under an atmosphere of nitrogen, and a solution of ethyl 3-(4-benzyloxyphenyl)-3-[N-(t-butoxycarbonyl)-N-methylamino]propionate (5.56 g, 13 mmol) obtained from Example 115a in tetrahydrofuran was slowly added thereto at −78° C. After stirr...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccccc1.c1ccccc1
HO-
O1CCCC1.O
0
0.5
CCOC(=O)CC(c1ccc(OCc2ccccc2)cc1)N(C)C(=O)OC(C)(C)C>O1CCCC1.O>CN(C(=O)OC(C)(C)C)C(CCO)c1ccc(OCc2ccccc2)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-70959b126ca245479646bacd142a7c3e
CN(C(=O)OC(C)(C)C)C(CCO)c1ccc(OCc2ccccc2)cc1.[C-]#N>>CN(C(=O)OC(C)(C)C)C(CCC#N)c1ccc(OCc2ccccc2)cc1
C1COCCOCCOCCOCCO1.C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CCO)N(C(OC(C)(C)C)=O)C.C(C)N(CC)CC.[C-]#N.[Na+].CS(=O)(=O)Cl>>C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CCC#N)N(C(OC(C)(C)C)=O)C
O[CH2:12][CH2:11][CH:10]([N:2]([CH3:1])[C:3](=[O:4])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9])[c:15]1[cH:16][cH:17][c:18]([O:19][CH2:20][c:21]2[cH:22][cH:23][cH:24][cH:25][cH:26]2)[cH:27][cH:28]1.[C-:13]#[N:14]>>[CH3:1][N:2]([C:3](=[O:4])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9])[CH:10]([CH2:11][CH2:12][C:13]#[N:14])[c:15]1[cH:16]...
CN(C(=O)OC(C)(C)C)C(CCO)c1ccc(OCc2ccccc2)cc1.[C-]#N
CN(C(=O)OC(C)(C)C)C(CCC#N)c1ccc(OCc2ccccc2)cc1
null
null
O1CCCC1
C-C Coupling
OtherReaction
a1e85c1b3a4aa1231f3779c2baa8b6951b270c05216d065e2aa7ce489240e0a5
1d32632fcc69ac04f0b8d96dc5305dd07d5339ab86bfe9a364cefb5e65c6d5b1
c1ccc(COc2ccccc2)cc1
O-[CH2;D2;+0:1]-[C:2]-[C:3].[C-;H0;D1:4]#[N;D1;H0:5]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[C;H0;D2;+0:4]#[N;D1;H0:5]
92.6
[{"value": 92.6, "product": "C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CCC#N)N(C(OC(C)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
t-Butyl N-[1-(4-benzyloxyphenyl)-3-hydroxypropyl]-N-methylcarbamate (1.50 g, 4.0 mmol) obtained from Example 115b was dissolved in tetrahydrofuran (20 ml) under an atmosphere of nitrogen. To the solution was added triethylamine (0.84 ml, 6.0 mmol) and then methanesulfonyl chloride (0.37 ml, 4.8 mmol), in an ice bath. T...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Nitrile
null
null
c1ccccc1.c1ccccc1
HO-
O1CCCC1
null
0.5
CN(C(=O)OC(C)(C)C)C(CCO)c1ccc(OCc2ccccc2)cc1.[C-]#N>O1CCCC1>CN(C(=O)OC(C)(C)C)C(CCC#N)c1ccc(OCc2ccccc2)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ca7ab29d47cf47ccb109611ba5a06c28
CN(C(=O)OC(C)(C)C)C(CCC#N)c1ccc(OCc2ccccc2)cc1>>CN(C(=O)OC(C)(C)C)C(CCCO)c1ccc(OCc2ccccc2)cc1
[H-].C(C(C)C)[Al+]CC(C)C.CCCCCC.[BH4-].[Na+].S(=O)(=O)([O-])[O-].[Na+].[Na+].C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CCC#N)N(C(OC(C)(C)C)=O)C>>C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CCCO)N(C(OC(C)(C)C)=O)C
N#[C:13][CH2:12][CH2:11][CH:10]([N:2]([CH3:1])[C:3](=[O:4])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9])[c:15]1[cH:16][cH:17][c:18]([O:19][CH2:20][c:21]2[cH:22][cH:23][cH:24][cH:25][cH:26]2)[cH:27][cH:28]1>>[CH3:1][N:2]([C:3](=[O:4])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9])[CH:10]([CH2:11][CH2:12][CH2:13][OH:14])[c:15]1[cH:16][cH:17...
CN(C(=O)OC(C)(C)C)C(CCC#N)c1ccc(OCc2ccccc2)cc1
CN(C(=O)OC(C)(C)C)C(CCCO)c1ccc(OCc2ccccc2)cc1
null
null
ClCCl.O
Functional Group Interconversion
OtherReaction
dfa6aab906f1cce8c060c3454d617eee54109b7fbe31f54f7240a7e17e9d9a0b
cfcea505f43817e62057efa9fa83f3ef47a11a99a8a6ad13903bd9b247dfd586
c1ccc(COc2ccccc2)cc1
N#[C;H0;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[O;D1;H1:4]
82.8
[{"value": 82.8, "product": "C(C1=CC=CC=C1)OC1=CC=C(C=C1)C(CCCO)N(C(OC(C)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
t-Butyl N-[1-(4-benzyloxyphenyl)-3-cyanopropyl]-N-methylcarbamate (1.00 g, 2.6 mmol) obtained from Example 115c was dissolved in dichloromethane (20 ml) under an atmosphere of nitrogen. To the solution was added 0.95 M solution of diisobutylaluminum hydride in hexane (5.5 ml, 5.3 mmol) at −78° C. and the temperature wa...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary alcohol
null
null
c1ccccc1.c1ccccc1
null
ClCCl.O
null
2
CN(C(=O)OC(C)(C)C)C(CCC#N)c1ccc(OCc2ccccc2)cc1>ClCCl.O>CN(C(=O)OC(C)(C)C)C(CCCO)c1ccc(OCc2ccccc2)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-1d5e32cdc1a24053b189723a5d5a0dca
CCOC(=O)C=C1NCCc2cc(OC)ccc21>>CCOC(=O)CC1NCCc2cc(OC)ccc21
COC=1C=C2CCNC(C2=CC1)=CC(=O)OCC.[OH-].[Na+].C([O-])([O-])=O.[K+].[K+]>>COC=1C=C2CCNC(C2=CC1)CC(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]=[C:7]1[NH:8][CH2:9][CH2:10][c:11]2[cH:12][c:13]([O:14][CH3:15])[cH:16][cH:17][c:18]21>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]1[NH:8][CH2:9][CH2:10][c:11]2[cH:12][c:13]([O:14][CH3:15])[cH:16][cH:17][c:18]21
CCOC(=O)C=C1NCCc2cc(OC)ccc21
CCOC(=O)CC1NCCc2cc(OC)ccc21
null
[Pt]=O
C(C)(=O)O
Reduction
Hydrogenation (double to single)
a2a16c1a99dc53e406de229794c537c379a76e9a646517a7c8ab052fadff31d4
b586296faf9080b398947dcba4825d3daf71a75997a309df19187f20bff3e49d
c1ccc2c(c1)CCNC2
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH;D2;+0:5]=[C;H0;D3;+0:6](-[#7:7]-[C:8])-[c:9](:[c:10]):[c:11]>>[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH2;D2;+0:5]-[CH;D3;+0:6](-[#7:7]-[C:8])-[c:9](:[c:10]):[c:11]
64
[{"value": 64.0, "product": "COC=1C=C2CCNC(C2=CC1)CC(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a solution of ethyl (6-methoxy-3,4-dihydro-2H-isoquinolin-1-yliden)-acetate (7.56 g) obtained in step (b) of Example 187 in acetic acid (50 ml) was added platinum oxide (400 mg), and the resulting mixture was stirred for 3 hours at room temperature under a hydrogen atmosphere. After stirring, the reaction mixture wa...
10.6084/m9.figshare.5104873.v1
null
Enamine
Ester
c1ccc2c(c1)CCNC2
c1ccc2c(c1)CCNC2
c1ccc2c(c1)CCNC2
null
[Pt]=O.C(C)(=O)O
null
3
CCOC(=O)C=C1NCCc2cc(OC)ccc21>[Pt]=O.C(C)(=O)O>CCOC(=O)CC1NCCc2cc(OC)ccc21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8511ca8f99834023b6fd94eef48cd1be
CCOC(=O)CC1c2ccc(O)cc2CCN1C(=O)OC(C)(C)C.CN(C)C(=O)Cl.O>>CCOC(=O)CC1C2=C(CCN1C(=O)OC(C)(C)C)CC(O)(OC(=O)N(C)C)C=C2
O.C(C)OC(=O)CC1N(CCC2=CC(=CC=C12)O)C(=O)OC(C)(C)C.C([O-])([O-])=O.[K+].[K+].CN(C(=O)Cl)C>>CN(C(=O)OC1(CC=2CCN(C(C2C=C1)CC(=O)OCC)C(=O)OC(C)(C)C)O)C
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]1[c:8]2[c:9]([cH:20][c:21]([OH:22])[cH:29][cH:30]2)[CH2:10][CH2:11][N:12]1[C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19].Cl[C:24](=[O:25])[N:26]([CH3:27])[CH3:28].[OH2:23]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]1[C:8]2=[C:9]([CH2:10][CH2:11][N:12]1[C:13](=[O:...
CCOC(=O)CC1c2ccc(O)cc2CCN1C(=O)OC(C)(C)C.CN(C)C(=O)Cl.O
CCOC(=O)CC1C2=C(CCN1C(=O)OC(C)(C)C)CC(O)(OC(=O)N(C)C)C=C2
null
null
CN(C=O)C
Protection
OtherReaction
6d2f16630df4090cd3c58cd2f34abacbdfcd8c38c0b22f845df91da04096e9d8
8113e1af9c36bbe7fed7499330e4e08640ab6a60502ef3feb1a2935ccf85500c
C1=CC2=C(CC1)CCNC2
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C;D1;H3:4])-[C;D1;H3:5].[#8:6]-[C:7](=[O;D1;H0:8])-[C:9]-[C:10]1-[#7:11](-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15](-[C;D1;H3:16])(-[C;D1;H3:17])-[C;D1;H3:18])-[C:19]-[C:20]-[c;H0;D3;+0:21]2:[cH;D2;+0:22]:[c;H0;D3;+0:23](-[O;D1;H1:24]):[cH;D2;+0:25]:[cH;D2;+0:26]:[c;H0;D3;+0:27]:2-1....
95
[{"value": 95.0, "product": "CN(C(=O)OC1(CC=2CCN(C(C2C=C1)CC(=O)OCC)C(=O)OC(C)(C)C)O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.5, "product": "CN(C(=O)OC1(CC=2CCN(C(C2C=C1)CC(=O)OCC)C(=O)OC(C)(C)C)O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2.5
HOUR
To a solution of t-butyl 1-ethoxycarbonylmethyl-6-hydroxy-3,4-dihydro-1H-isoquinoline-2-carboxylate (1.70 g, 5.07 mmol) synthesized in step (d) of Example 187 in dimethylformamide (5 ml) were added potassium carbonate (1.03 g, 7.50 mmol) and N,N-dimethylcarbamoyl chloride (0.69 ml, 7.5 mmol), and the resulting mixture ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Tertiary amide.Aromatic alcohol
Carbamic ester.Ether.Tertiary alcohol
c1ccc2c(c1)CC[NH]C2
C1=CC2=C(CC1)CC[NH]C2
C1=CC2=C(CC1)CC[NH]C2
HCl
CN(C=O)C
null
2.5
CCOC(=O)CC1c2ccc(O)cc2CCN1C(=O)OC(C)(C)C.CN(C)C(=O)Cl.O>CN(C=O)C>CCOC(=O)CC1C2=C(CCN1C(=O)OC(C)(C)C)CC(O)(OC(=O)N(C)C)C=C2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-49eed0ece98a4e43bb1fdcb2d99d8533
CCOC(=O)CC1C2=C(CCN1C(=O)OC(C)(C)C)CC(O)(OC(=O)N(C)C)C=C2>>CN(C)C(=O)Oc1ccc2c(c1)CCN(C(=O)OC(C)(C)C)C2CCO
CN(C(=O)OC1(CC=2CCN(C(C2C=C1)CC(=O)OCC)C(=O)OC(C)(C)C)O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+].O>>CN(C(=O)OC=1C=C2CCN(C(C2=CC1)CCO)C(=O)OC(C)(C)C)C
CCO[C:25]([CH2:24][CH:23]1[C:10]2=[C:11]([CH2:12][C:7](O)([O:6][C:4]([N:2]([CH3:1])[CH3:3])=[O:5])[CH:8]=[CH:9]2)[CH2:13][CH2:14][N:15]1[C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:26]>>[CH3:1][N:2]([CH3:3])[C:4](=[O:5])[O:6][c:7]1[cH:8][cH:9][c:10]2[c:11]([cH:12]1)[CH2:13][CH2:14][N:15]([C:16](=[O:17])[...
CCOC(=O)CC1C2=C(CCN1C(=O)OC(C)(C)C)CC(O)(OC(=O)N(C)C)C=C2
CN(C)C(=O)Oc1ccc2c(c1)CCN(C(=O)OC(C)(C)C)C2CCO
null
null
O1CCCC1
Reduction
OtherReaction
3853f56c6f0ecde368d58bc22fc3494232d8f07bad3b0cd3580c749ca6f02671
f97908a80f5a6be714b164c5d0248e40307dea320152935297423c15a42639b6
c1ccc2c(c1)CCNC2
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]-[C:4]1-[#7:5](-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12])-[C:13]-[C:14]-[C;H0;D3;+0:15]2=[C;H0;D3;+0:16]-1-[CH;D2;+0:17]=[CH;D2;+0:18]-[C;H0;D4;+0:19](-O)(-[#8:20]-[C:21](-[#7:22])=[O;D1;H0:23])-[CH2;D2;+0:24]-2>>[#7:22]-[C:21](=[O;D1;H0:23])...
78.2
[{"value": 78.0, "product": "CN(C(=O)OC=1C=C2CCN(C(C2=CC1)CCO)C(=O)OC(C)(C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.2, "product": "CN(C(=O)OC=1C=C2CCN(C(C2=CC1)CCO)C(=O)OC(C)(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
20
MINUTE
To a solution of t-butyl 6-dimethylcarbamoyloxy-1-ethoxycarbonylmethyl-6-hydroxy-3,4-dihydro-1H-isoquinoline-2-carboxylate (1.97 g, 4.84 mmol) synthesized in step (e) of Example 187 in tetrahydrofuran (30 ml) was added lithium aluminum hydride (270 mg, 7.2 mmol) at −78° C., and the resulting mixture was stirred for 20 ...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether.Tertiary alcohol
Ether.Primary alcohol
C1=CC2=C(CC1)CC[NH]C2
c1ccc2c(c1)CC[NH]C2
c1ccc2c(c1)CC[NH]C2
HO-
O1CCCC1
0
0.333333
CCOC(=O)CC1C2=C(CCN1C(=O)OC(C)(C)C)CC(O)(OC(=O)N(C)C)C=C2>O1CCCC1>CN(C)C(=O)Oc1ccc2c(c1)CCN(C(=O)OC(C)(C)C)C2CCO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-810f16b7ef66497bb4aef6c797da3d2b
COc1ccc2c(c1)CCN[C@@H]2CCO[Si](C)(C)C(C)(C)C>>COc1ccc2c(c1)CCN[C@@H]2CCO
COC=1C=C2CCN[C@@H](C2=CC1)CCO[Si](C)(C)C(C)(C)C.FC(C(=O)N)(F)F.F.O.C(O)([O-])=O.[Na+]>>COC=1C=C2CCN[C@@H](C2=CC1)CCO.FC(C(=O)N)(F)F
CC(C)(C)[Si](C)(C)[O:15][CH2:14][CH2:13][C@@H:12]1[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8][c:7]2[CH2:9][CH2:10][NH:11]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[CH2:9][CH2:10][NH:11][C@@H:12]2[CH2:13][CH2:14][OH:15]
COc1ccc2c(c1)CCN[C@@H]2CCO[Si](C)(C)C(C)(C)C
COc1ccc2c(c1)CCN[C@@H]2CCO
null
null
C(C)#N
Deprotection
Alcohol deprotection from silyl ethers
6ff8c9c41093ab5237b871dd4689ba6431022d615e227d3774901a983c846e4b
84d9f5b4e7757c58e584c26c7d52c9a3f594fbcb0c0d22f34765a93a932fcd5b
c1ccc2c(c1)CCNC2
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[OH;D1;+0:1]
79
[{"value": 79.0, "product": "COC=1C=C2CCN[C@@H](C2=CC1)CCO.FC(C(=O)N)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 74.3, "product": "COC=1C=C2CCN[C@@H](C2=CC1)CCO.FC(C(=O)N)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 6-methoxy-1-(R)-(2-t-butyldimethylsilyloxyethyl)-3,4-dihydro-1H-isoquinoline-trifluoroacetamide (1.14 g, 2.73 mmol) obtained in step (a) of Example 190 in acetonitrile (10 ml) was added dropwise 48% solution of hydrofluoric acid in water (0.5 ml, 13.67 mmol) gradually with stirring under cooling in a w...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Primary alcohol
null
null
c1ccc2c(c1)CCNC2
Other
C(C)#N
null
null
COc1ccc2c(c1)CCN[C@@H]2CCO[Si](C)(C)C(C)(C)C>C(C)#N>COc1ccc2c(c1)CCN[C@@H]2CCO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-04725603260849d48bb508a803e3335e
BrC(Br)(Br)Br.COc1ccc2c(c1)CCN[C@@H]2CCO>>COc1ccc2c(c1)CCN[C@@H]2CCBr
COC=1C=C2CCN[C@@H](C2=CC1)CCO.FC(C(=O)N)(F)F.C(Br)(Br)(Br)Br.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>COC=1C=C2CCN[C@@H](C2=CC1)CCBr.FC(C(=O)N)(F)F
BrC(Br)(Br)[Br:15].O[CH2:14][CH2:13][C@@H:12]1[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8][c:7]2[CH2:9][CH2:10][NH:11]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[CH2:9][CH2:10][NH:11][C@@H:12]2[CH2:13][CH2:14][Br:15]
BrC(Br)(Br)Br.COc1ccc2c(c1)CCN[C@@H]2CCO
COc1ccc2c(c1)CCN[C@@H]2CCBr
null
null
ClCCl
Functional Group Interconversion
Appel reaction
752e1807cd47d8316010cc3f92eab16c5a89ffb844d9514fcae469ba993c78dd
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
c1ccc2c(c1)CCNC2
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3]-[C:4]-[#7:5]>>[#7:5]-[C:4]-[C:3]-[CH2;D2;+0:2]-[Br;H0;D1;+0:1]
98
[{"value": 98.0, "product": "COC=1C=C2CCN[C@@H](C2=CC1)CCBr.FC(C(=O)N)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.4, "product": "COC=1C=C2CCN[C@@H](C2=CC1)CCBr.FC(C(=O)N)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 6-methoxy-1-(R)-(2-hydroxyethyl)-3,4-dihydro-1H-isoquinoline-trifluoroacetamide (330 mg, 1.09 mmol) obtained in step (b) of Example 190 and carbon tetrabromide (542 mg, 1.63 mmol) in dichloromethane (5 ml) was added gradually triphenyl phosphine (343 mg, 1.31 mmol) with stirring under cooling in a wate...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
null
null
c1ccc2c(c1)CCNC2
HBr
ClCCl
null
null
BrC(Br)(Br)Br.COc1ccc2c(c1)CCN[C@@H]2CCO>ClCCl>COc1ccc2c(c1)CCN[C@@H]2CCBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-65d431d7209b45498ff11f66c2e891a5
COc1ccc2c(c1)CCN[C@@H]2CCBr>>Oc1ccc2c(c1)CCN[C@@H]2CCBr
C(O)([O-])=O.[Na+].COC=1C=C2CCN[C@@H](C2=CC1)CCBr.FC(C(=O)N)(F)F.B(Br)(Br)Br>>OC=1C=C2CCN[C@@H](C2=CC1)CCBr.FC(C(=O)N)(F)F
C[O:8][c:9]1[cH:10][cH:11][c:12]2[c:13]([cH:14]1)[CH2:15][CH2:16][NH:17][C@@H:18]2[CH2:19][CH2:20][Br:21]>>[OH:8][c:9]1[cH:10][cH:11][c:12]2[c:13]([cH:14]1)[CH2:15][CH2:16][NH:17][C@@H:18]2[CH2:19][CH2:20][Br:21]
COc1ccc2c(c1)CCN[C@@H]2CCBr
Oc1ccc2c(c1)CCN[C@@H]2CCBr
null
null
ClCCl
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1ccc2c(c1)CCNC2
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
75
[{"value": 75.0, "product": "OC=1C=C2CCN[C@@H](C2=CC1)CCBr.FC(C(=O)N)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 70.9, "product": "OC=1C=C2CCN[C@@H](C2=CC1)CCBr.FC(C(=O)N)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 6-methoxy-1-(R)-(2-bromoethyl)-3,4-dihydro-1H-isoquinoline-trifluoroacetamide (390 mg, 1.07 mmol) obtained in step (c) of Example 190 in dichloromethane (5 ml) was added 1M solution of boron tribromide in dichloromethane (2.14 ml, 2.14 mmol) gradually at −78° C. with stirring. The resulting mixture was...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccc2c(c1)CCNC2
Other
ClCCl
null
null
COc1ccc2c(c1)CCN[C@@H]2CCBr>ClCCl>Oc1ccc2c(c1)CCN[C@@H]2CCBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-55e5a9fd7546411f9c81bab5cdc86e74
CN(C)C(=O)Cl.Oc1ccc2c(c1)CCN[C@@H]2CCBr>>CN(C)C(=O)Oc1ccc2c(c1)CCN[C@@H]2CCBr
O.OC=1C=C2CCN[C@@H](C2=CC1)CCBr.FC(C(=O)N)(F)F.C([O-])([O-])=O.[K+].[K+].CN(C(=O)Cl)C>>CN(C(=O)OC=1C=C2CCN[C@@H](C2=CC1)CCBr)C.FC(C(=O)N)(F)F
Cl[C:4]([N:2]([CH3:1])[CH3:3])=[O:5].[OH:6][c:7]1[cH:8][cH:9][c:10]2[c:11]([cH:12]1)[CH2:13][CH2:14][NH:15][C@@H:16]2[CH2:17][CH2:18][Br:19]>>[CH3:1][N:2]([CH3:3])[C:4](=[O:5])[O:6][c:7]1[cH:8][cH:9][c:10]2[c:11]([cH:12]1)[CH2:13][CH2:14][NH:15][C@@H:16]2[CH2:17][CH2:18][Br:19]
CN(C)C(=O)Cl.Oc1ccc2c(c1)CCN[C@@H]2CCBr
CN(C)C(=O)Oc1ccc2c(c1)CCN[C@@H]2CCBr
null
null
CN(C=O)C
Protection
Schotten-Baumann to ester
76fc23af07d8d02fec539138b5d326dfd4e833212bae1d173120f54983c8b7d8
4c7d92b589147a4e2aa8407ff52bd0eb1be84bdb6595779d27beb0c5d6fdd0e2
c1ccc2c(c1)CCNC2
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C;D1;H3:4])-[C;D1;H3:5].[OH;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[C;D1;H3:4]-[#7:3](-[C;D1;H3:5])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[O;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]
52
[{"value": 52.0, "product": "CN(C(=O)OC=1C=C2CCN[C@@H](C2=CC1)CCBr)C.FC(C(=O)N)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 50.1, "product": "CN(C(=O)OC=1C=C2CCN[C@@H](C2=CC1)CCBr)C.FC(C(=O)N)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 6-hydroxy-1-(R)-(2-bromoethyl)-3,4-dihydro-1H-isoquinoline-trifluoroacetamide (270 mg, 0.77 mmol) obtained in step (d) of Example 190 and potassium carbonate (268 mg, 1.94 mmol) in dimethylformamide (3 ml) was added dimethylcarbamyl chloride (0.2 ml, 1.55 mmol) gradually with stirring under cooling in ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Tertiary amide.Aromatic alcohol
Carbamic ester
null
null
c1ccc2c(c1)CCNC2
HCl
CN(C=O)C
null
null
CN(C)C(=O)Cl.Oc1ccc2c(c1)CCN[C@@H]2CCBr>CN(C=O)C>CN(C)C(=O)Oc1ccc2c(c1)CCN[C@@H]2CCBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-cf323f7afa53467cafe4b857cd8596b7
CN(C)C(=O)Oc1ccc2c(c1)CCN[C@@H]2CCBr.Cc1cc(O)ccc1Cl>>Cc1cc(OCC[C@H]2NCCc3cc(OC(=O)N(C)C)ccc32)ccc1Cl
C([O-])([O-])=O.[K+].[K+].[I-].[K+].ClC=1C(=CC(=CC1)O)C.CN(C(=O)OC=1C=C2CCN[C@@H](C2=CC1)CCBr)C.FC(C(=O)N)(F)F>>CN(C(=O)OC=1C=C2CCN[C@@H](C2=CC1)CCOC1=CC(=C(C=C1)Cl)C)C.FC(C(=O)N)(F)F
Br[CH2:6][CH2:7][C@H:8]1[NH:9][CH2:10][CH2:11][c:12]2[cH:13][c:14]([O:15][C:16](=[O:17])[N:18]([CH3:19])[CH3:20])[cH:21][cH:22][c:23]21.[CH3:1][c:2]1[cH:3][c:4]([OH:5])[cH:24][cH:25][c:26]1[Cl:27]>>[CH3:1][c:2]1[cH:3][c:4]([O:5][CH2:6][CH2:7][C@H:8]2[NH:9][CH2:10][CH2:11][c:12]3[cH:13][c:14]([O:15][C:16](=[O:17])[N:18]...
CN(C)C(=O)Oc1ccc2c(c1)CCN[C@@H]2CCBr.Cc1cc(O)ccc1Cl
Cc1cc(OCC[C@H]2NCCc3cc(OC(=O)N(C)C)ccc32)ccc1Cl
null
null
O.CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccc(OCC[C@H]2NCCc3ccccc32)cc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3]-[#7:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[#7:4]-[C:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]
84
[{"value": 84.0, "product": "CN(C(=O)OC=1C=C2CCN[C@@H](C2=CC1)CCOC1=CC(=C(C=C1)Cl)C)C.FC(C(=O)N)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 80.7, "product": "CN(C(=O)OC=1C=C2CCN[C@@H](C2=CC1)CCOC1=CC(=C(C=C1)Cl)C)C.FC(C(=O)N)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of potassium carbonate (115 mg, 0.83 mmol), potassium iodide (catalytic amount) and 4-chloro-m-cresol (65 mg, 0.46 mmol) in dimethylformamide (2 ml) was added a solution of 6-dimethylcarbamoyloxy-1-(R)-(2-bromoethyl)-3,4-dihydro-1H-isoquinoline-trifluoroacetamide (160 mg, 0.38 mmol) obtained in step (e) o...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1.c1ccc2c(c1)CCNC2
HBr
O.CN(C=O)C
null
null
CN(C)C(=O)Oc1ccc2c(c1)CCN[C@@H]2CCBr.Cc1cc(O)ccc1Cl>O.CN(C=O)C>Cc1cc(OCC[C@H]2NCCc3cc(OC(=O)N(C)C)ccc32)ccc1Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-f82cb094b916404d816fa1996624d2f5
CN(C)C(=O)Cl.O=Cc1ccc(O)cc1O>>CN(C)C(=O)Oc1ccc(C=O)c(O)c1
[H-].[Na+].OC1=C(C=O)C=CC(=C1)O.CN(C(=O)Cl)C>>CN(C(OC1=CC(=C(C=C1)C=O)O)=O)C
Cl[C:4]([N:2]([CH3:1])[CH3:3])=[O:5].[OH:6][c:7]1[cH:8][cH:9][c:10]([CH:11]=[O:12])[c:13]([OH:14])[cH:15]1>>[CH3:1][N:2]([CH3:3])[C:4](=[O:5])[O:6][c:7]1[cH:8][cH:9][c:10]([CH:11]=[O:12])[c:13]([OH:14])[cH:15]1
CN(C)C(=O)Cl.O=Cc1ccc(O)cc1O
CN(C)C(=O)Oc1ccc(C=O)c(O)c1
null
null
O
Protection
Schotten-Baumann to ester
76fc23af07d8d02fec539138b5d326dfd4e833212bae1d173120f54983c8b7d8
4c7d92b589147a4e2aa8407ff52bd0eb1be84bdb6595779d27beb0c5d6fdd0e2
c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C;D1;H3:4])-[C;D1;H3:5].[OH;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[C;D1;H3:4]-[#7:3](-[C;D1;H3:5])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[O;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]
30
[{"value": 30.0, "product": "CN(C(OC1=CC(=C(C=C1)C=O)O)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 29.7, "product": "CN(C(OC1=CC(=C(C=C1)C=O)O)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a suspension of sodium hydride (5.74 g, 239 mmol), which was prepared free from mineral oil by washing with hexane, in dimethylformamide (100 ml) was added 2,4-dihydroxybenzaldehyde (15.0 g, 109 mmol) at 0° C. with stirring, and the resulting mixture was stirred for 30 minutes at 0° C. under a nitrogen atmosphere. S...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Tertiary amide.Aromatic alcohol
Carbamic ester
null
null
c1ccccc1
HCl
O
null
null
CN(C)C(=O)Cl.O=Cc1ccc(O)cc1O>O>CN(C)C(=O)Oc1ccc(C=O)c(O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-6ebe0a412cc846918196e16ac99face6
C=[CH][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.CN(C)C(=O)Oc1ccc(C=O)c(OS(=O)(=O)C(F)(F)F)c1>>C=Cc1cc(OC(=O)N(C)C)ccc1C=O
[F-].[K+].FC(S(=O)(=O)OC1=C(C=CC(=C1)OC(N(C)C)=O)C=O)(F)F.[Cl-].[Li+].C(CCC)[Sn](C=C)(CCCC)CCCC>>CN(C(OC1=CC(=C(C=C1)C=O)C=C)=O)C
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH:2]=[CH2:1].O=S(=O)(O[c:3]1[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[CH3:11])[cH:12][cH:13][c:14]1[CH:15]=[O:16])C(F)(F)F>>[CH2:1]=[CH:2][c:3]1[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[CH3:11])[cH:12][cH:13][c:14]1[CH:15]=[O:16]
C=[CH][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.CN(C)C(=O)Oc1ccc(C=O)c(OS(=O)(=O)C(F)(F)F)c1
C=Cc1cc(OC(=O)N(C)C)ccc1C=O
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.C(C)(C)(C)C1=C(C(=CC=C1)C(C)(C)C)O
O1CCOCC1
C-C Coupling
Stille reaction_vinyl OTf
19b30501d1aaa5f5dd56b13112130366c0e45d6c2d2ca2c3e4e656b3de7ef26d
22963776d86934928a954d267e6c7c5a64095fcc3303c473fde6e3c4d4878a47
c1ccccc1
C-C-C-[CH2]-[Sn](-[CH2]-C-C-C)(-[CH2]-C-C-C)-[CH;D2;+0:1]=[C;D1;H2:2].F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:3](:[c:4]:[c:5]):[c:6](-[C:7]=[O;D1;H0:8]):[c:9]>>[C;D1;H2:2]=[CH;D2;+0:1]-[c;H0;D3;+0:3](:[c:4]:[c:5]):[c:6](-[C:7]=[O;D1;H0:8]):[c:9]
79.5
[{"value": 79.0, "product": "CN(C(OC1=CC(=C(C=C1)C=O)C=C)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.5, "product": "CN(C(OC1=CC(=C(C=C1)C=O)C=C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 5-dimethylcarbamoyloxy-2-formyl-phenyl trifluoromethanesulfonate (4.13 g, 12.1 mmol) obtained in step (b) of Example 192 in 1,4-dioxane (15 ml) were added tetrakis(triphenylphosphine)palladium (693 mg, 0.600 mmol), 2,6-di-t-butylphenol (5 mg), lithium chloride (1.54 g, 36.4 mmol) and tributyl(vinyl)tin...
10.6084/m9.figshare.5104873.v1
null
Triflate.Vinyl.Tin
Vinyl
c1ccccc1
c1ccccc1
c1ccccc1
TfOH.HO-.Sn
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.C(C)(C)(C)C1=C(C(=CC=C1)C(C)(C)C)O.O1CCOCC1
null
null
C=[CH][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.CN(C)C(=O)Oc1ccc(C=O)c(OS(=O)(=O)C(F)(F)F)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.C(C)(C)(C)C1=C(C(=CC=C1)C(C)(C)C)O.O1CCOCC1>C=Cc1cc(OC(=O)N(C)C)c...
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-fa43c8d32bb7464c940f3914b41e2b99
C=Cc1cc(OC(=O)N(C)C)ccc1C=O.CCOC(C)=O>>C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CC(=O)OCC
CN(C(OC1=CC(=C(C=C1)C=O)C=C)=O)C.[Cl-].[NH4+].C(C)(C)NC(C)C.C(CCC)[Li].CCCCCC.C(C)(=O)OCC>>CN(C(=O)OC1=CC(=C(C=C1)C(CC(=O)OCC)O)C=C)C
[CH2:1]=[CH:2][c:3]1[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[CH3:11])[cH:12][cH:13][c:14]1[CH:15]=[O:16].[CH3:17][C:18](=[O:19])[O:20][CH2:21][CH3:22]>>[CH2:1]=[CH:2][c:3]1[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[CH3:11])[cH:12][cH:13][c:14]1[CH:15]([OH:16])[CH2:17][C:18](=[O:19])[O:20][CH2:21][CH3:22]
C=Cc1cc(OC(=O)N(C)C)ccc1C=O.CCOC(C)=O
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CC(=O)OCC
null
null
O1CCCC1
C-C Coupling
OtherReaction
5c727118385c562f285df4622fd28beee54f2a6dc613daeca0713283cec89087
12ce375342f37362e14813852abaca485261821306a77d2d6bbedf8a6a5866f3
c1ccccc1
[C;D1;H2:1]=[C:2]-[c:3]:[c:4](-[CH;D2;+0:5]=[O;H0;D1;+0:6]):[c:7].[C:8]-[#8:9]-[C:10](-[CH3;D1;+0:11])=[O;D1;H0:12]>>[C:8]-[#8:9]-[C:10](=[O;D1;H0:12])-[CH2;D2;+0:11]-[CH;D3;+0:5](-[OH;D1;+0:6])-[c:4](:[c:7]):[c:3]-[C:2]=[C;D1;H2:1]
99.8
[{"value": 99.0, "product": "CN(C(=O)OC1=CC(=C(C=C1)C(CC(=O)OCC)O)C=C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.8, "product": "CN(C(=O)OC1=CC(=C(C=C1)C(CC(=O)OCC)O)C=C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of diisopropylamine (1.26 g, 12.5 mmol) in tetrahydrofuran (30 ml) was added 1.6M solution of n-butyllithium in hexane (7.20 ml, 11.5 mmol) at −20° C. with stirring, and the resulting mixture was stirred for 20 minutes at −20° C. under a nitrogen atmosphere. Subsequently, ethyl acetate (1.07 ml, 11.0 mmol...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester
Ester.Secondary alcohol
null
null
c1ccccc1
null
O1CCCC1
null
null
C=Cc1cc(OC(=O)N(C)C)ccc1C=O.CCOC(C)=O>O1CCCC1>C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CC(=O)OCC
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2fb639fd66584ac792fd3c6665db98e8
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CC(=O)OCC>>C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO
O.Cl.CN(C(=O)OC1=CC(=C(C=C1)C(CC(=O)OCC)O)C=C)C.[BH4-].[Li+]>>CN(C(OC1=CC(=C(C=C1)C(CCO)O)C=C)=O)C
CCO[C:18]([CH2:17][CH:15]([c:14]1[c:3]([CH:2]=[CH2:1])[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[CH3:11])[cH:12][cH:13]1)[OH:16])=[O:19]>>[CH2:1]=[CH:2][c:3]1[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[CH3:11])[cH:12][cH:13][c:14]1[CH:15]([OH:16])[CH2:17][CH2:18][OH:19]
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CC(=O)OCC
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO
null
null
O1CCCC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccccc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]-[C:4]>>[C:4]-[C:3]-[CH2;D2;+0:1]-[OH;D1;+0:2]
97.3
[{"value": 97.0, "product": "CN(C(OC1=CC(=C(C=C1)C(CCO)O)C=C)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.3, "product": "CN(C(OC1=CC(=C(C=C1)C(CCO)O)C=C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of ethyl 3-(4-dimethylcarbamoyloxy-2-vinyl-phenyl)-3-hydroxy-propionate (5.28 g, 17.2 mmol) obtained in step (d) of Example 192 in tetrahydrofuran (50 ml) was added lithium tetrahydroborate (544 mg, 25.0 mmol) at −20° C. with stirring, and the reaction temperature was raised gradually to ambient temperatu...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccccc1
HO-
O1CCCC1
null
null
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CC(=O)OCC>O1CCCC1>C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-fa7e08c51f0d436a83a30c39cd26cb99
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO.CC(C)(C)[Si](C)(C)Cl.CCN(CC)CC>>C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
O.CN(C(OC1=CC(=C(C=C1)C(CCO)O)C=C)=O)C.C(C)N(CC)CC.C(C)(C)(C)[Si](Cl)(C)C>>CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)O)C=C)=O)C
[CH2:1]=[CH:2][c:3]1[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[CH3:11])[cH:12][cH:13][c:14]1[CH:15]([OH:16])[CH2:17][CH2:18][OH:19].Cl[Si:20]([CH3:21])([CH3:27])[C:33]([CH3:34])([CH3:35])[CH3:36].N([CH2:22][CH3:25])([CH2:29][CH3:30])[CH2:32][CH3:31]>>[CH2:1]=[CH:2][c:3]1[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[...
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO.CC(C)(C)[Si](C)(C)Cl.CCN(CC)CC
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
null
CN(C1=CC=NC=C1)C
ClCCl
Aromatic Heterocycle Formation
OtherReaction
500aab33a5fdae74a8362d9d6c793395a5801abb4ca2c4d3e1d2b2517e0a3aef
9209b2acefe19f140772464284a8330dc3debcbdc34c49c2add1f0a0e951600b
c1ccc(CCCO[SiH](c2ccccc2)c2ccccc2)cc1
Cl-[Si;H0;D4;+0:1](-[CH3;D1;+0:2])(-[CH3;D1;+0:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7].[CH3;D1;+0:8]-[CH2;D2;+0:9]-N(-[CH2;D2;+0:10]-[CH3;D1;+0:11])-[CH2;D2;+0:12]-[CH3;D1;+0:13].[C:14]-[C:15]-[OH;D1;+0:16]>>[C:14]-[C:15]-[O;H0;D2;+0:16]-[Si;H0;D4;+0:1](-[c;H0;D3;+0:2]1:[c:17]:[cH;D2;+0:8]:[c:18]:[c:19]:[cH;D...
139.6
[{"value": 70.0, "product": "CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)O)C=C)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 139.6, "product": "CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)O)C=C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
To a solution of 4-(1,3-dihydroxy-propyl)-3-vinyl-phenyl dimethylcarbamate (4.44 g, 16.7 mmol) synthesized in step (e) of Example 192 in dichloromethane (40 ml) were added triethylamine (4.18 ml, 30.0 mmol), t-butyldimethylchlorosilane (4.67 g, 17.0 mmol) and a catalytic amount of 4-dimethylaminopyridine at −0° C. with...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Tertiary amine.Silyl protective group
Silyl protective group
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1
HCl
CN(C1=CC=NC=C1)C.ClCCl
null
5
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO.CC(C)(C)[Si](C)(C)Cl.CCN(CC)CC>CN(C1=CC=NC=C1)C.ClCCl>C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-bbad98721f0c4cb7b111c662fc92423b
BrC(Br)(Br)Br.C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C>>C=Cc1cc(OC(=O)N(C)C)ccc1C(O)(Br)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)O)C=C)=O)C.C(Br)(Br)(Br)Br.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)(O)Br)C=C)=O)C
BrC(Br)(Br)[Br:17].[CH2:1]=[CH:2][c:3]1[cH:4][c:5]([O:6][C:7](=[O:8])[N:9]([CH3:10])[CH3:11])[cH:12][cH:13][c:14]1[CH:15]([OH:16])[CH2:18][CH2:19][O:20][Si:21]([c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1)([c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1)[C:34]([CH3:35])([CH3:36])[CH3:37]>>[CH2:1]=[CH:2][c:3]1[cH:4][c:5]([O:...
BrC(Br)(Br)Br.C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
C=Cc1cc(OC(=O)N(C)C)ccc1C(O)(Br)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
null
null
ClCCl
Functional Group Interconversion
Bromination
9f0ae5e83907ecc1fcfb1d88ad36f98595319ee8517fc263e77784e52e82e13b
f5672e6730ea422d01df5937ff46c934f5dfdf1d4fbf514db56d670518e21c21
c1ccc(CCCO[SiH](c2ccccc2)c2ccccc2)cc1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].[C:2]-[C:3]-[CH;D3;+0:4](-[O;D1;H1:5])-[c:6](:[c:7]):[c:8]-[C:9]=[C;D1;H2:10]>>[Br;H0;D1;+0:1]-[C;H0;D4;+0:4](-[O;D1;H1:5])(-[C:3]-[C:2])-[c:6](:[c:7]):[c:8]-[C:9]=[C;D1;H2:10]
78
[{"value": 78.0, "product": "CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)(O)Br)C=C)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.6, "product": "CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)(O)Br)C=C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": f...
null
null
1
HOUR
To a solution of 4-[3-(t-butyl-diphenyl-silanyloxy)-1-hydroxy-propyl]-3-vinyl-phenyl dimethylcarbamate (3.00 g, 5.95 mmol) synthesized in step (f) of Example 192 and carbon tetrabromide (3.98 g, 12.0 mmol) in dichloromethane (20 ml) was added triphenyl phosphine (3.14 g, 12.0 mmol) at room temperature, and the resultin...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Secondary alcohol
Tertiary halide
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HBr
ClCCl
null
1
BrC(Br)(Br)Br.C=Cc1cc(OC(=O)N(C)C)ccc1C(O)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C>ClCCl>C=Cc1cc(OC(=O)N(C)C)ccc1C(O)(Br)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-61bb9b670573410ba6523b2a8e732d6d
C=CCN.C=Cc1cc(OC(=O)N(C)C)ccc1C(O)(Br)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C>>C=CCNC(O)(CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C)c1ccc(OC(=O)N(C)C)cc1C=C
CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)(O)Br)C=C)=O)C.C(C=C)N>>CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)(O)NCC=C)C=C)=O)C
[CH2:1]=[CH:2][CH2:3][NH2:4].Br[C:5]([OH:6])([CH2:7][CH2:8][O:9][Si:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[C:23]([CH3:24])([CH3:25])[CH3:26])[c:27]1[cH:28][cH:29][c:30]([O:31][C:32](=[O:33])[N:34]([CH3:35])[CH3:36])[cH:37][c:38]1[CH:39]=[CH2:40]>>[CH2:1]=[CH:2][CH2...
C=CCN.C=Cc1cc(OC(=O)N(C)C)ccc1C(O)(Br)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
C=CCNC(O)(CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C)c1ccc(OC(=O)N(C)C)cc1C=C
null
null
C(C)#N
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
07af7d4c7984f572726ef942df12a89735b132164a86a1c8a3ba0c5326426194
1eca3e4a42a47a41a21e5d78efdcb9eebb24be6eecab751fa86ecd6c304b18a3
c1ccc(CCCO[SiH](c2ccccc2)c2ccccc2)cc1
Br-[C;H0;D4;+0:1](-[O;D1;H1:2])(-[C:3]-[C:4])-[c:5](:[c:6]):[c:7]-[C:8]=[C;D1;H2:9].[C;D1;H2:10]=[C:11]-[C:12]-[NH2;D1;+0:13]>>[C:4]-[C:3]-[C;H0;D4;+0:1](-[O;D1;H1:2])(-[NH;D2;+0:13]-[C:12]-[C:11]=[C;D1;H2:10])-[c:5](:[c:6]):[c:7]-[C:8]=[C;D1;H2:9]
72
[{"value": 72.0, "product": "CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)(O)NCC=C)C=C)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 70.5, "product": "CN(C(OC1=CC(=C(C=C1)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)(O)NCC=C)C=C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desir...
null
null
8
HOUR
To a solution of 4-[1-bromo-3-(t-butyl-diphenyl-silanyloxy)-1-hydroxy-propyl]-3-vinyl-phenyl dimethylcarbamate (2.62 g, 4.62 mmol) synthesized in step (g) of Example 192 in acetonitrile (20 ml) was added allylamine (1.87 ml, 25.0 mmol) at room temperature, and the resulting mixture was stirred at room temperature overn...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary alcohol.Primary amine
Tertiary alcohol.Secondary amine
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HBr
C(C)#N
null
8
C=CCN.C=Cc1cc(OC(=O)N(C)C)ccc1C(O)(Br)CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C>C(C)#N>C=CCNC(O)(CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C)c1ccc(OC(=O)N(C)C)cc1C=C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-31e19f1e653e4f18a99319eceab0f633
C=CCN(C(=O)OC(C)(C)C)C(CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C)c1ccc(OC(=O)N(C)C)cc1C=C>>CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
C(C=C)N(C(OC(C)(C)C)=O)C(CCO[Si](C1=CC=CC=C1)(C1=CC=CC=C1)C(C)(C)C)C1=C(C=C(C=C1)OC(N(C)C)=O)C=C>>C(C)(C)(C)[Si](OCCC1N(CC=CC2=C1C=CC(=C2)OC(N(C)C)=O)C(=O)OC(C)(C)C)(C2=CC=CC=C2)C2=CC=CC=C2
C=[CH:13][c:11]1[c:10]([CH:24]([N:16]([CH2:15][CH:14]=C)[C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[CH2:25][CH2:26][O:27][Si:28]([c:29]2[cH:30][cH:31][cH:32][cH:33][cH:34]2)([c:35]2[cH:36][cH:37][cH:38][cH:39][cH:40]2)[C:41]([CH3:42])([CH3:43])[CH3:44])[cH:9][cH:8][c:7]([O:6][C:4]([N:2]([CH3:1])[CH3:3])=[O...
C=CCN(C(=O)OC(C)(C)C)C(CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C)c1ccc(OC(=O)N(C)C)cc1C=C
CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
null
CC1=CC(=C(C(=C1)C)N2CCN([CH-]2)C3=C(C=C(C=C3C)C)C)C.C1CCC(CC1)[PH+](C2CCCCC2)C3CCCCC3.C1=CC=C(C=C1)C=[Ru](Cl)Cl
ClCCl
C-C Coupling
OtherReaction
234a9f25d5c12ce6762f8b70a6ea1ebc56ad581f8e23f3c9a3e6209e4c8c40c9
7cc827c291e2a977a7a91dfb00752230897a77bed46038b3e1551b560ca4b6fc
C1=Cc2ccccc2C(CCO[SiH](c2ccccc2)c2ccccc2)NC1
C=[CH;D2;+0:1]-[C:2]-[#7:3]-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7](-[C;D1;H3:8])(-[C;D1;H3:9])-[C;D1;H3:10].C=[CH;D2;+0:11]-[c:12](:[c:13]):[c:14]>>[C;D1;H3:8]-[C:7](-[C;D1;H3:9])(-[C;D1;H3:10])-[#8:6]-[C:4](=[O;D1;H0:5])-[#7:3]-[C:2]-[CH;D2;+0:1]=[CH;D2;+0:11]-[c:12](:[c:13]):[c:14]
96
[{"value": 96.0, "product": "C(C)(C)(C)[Si](OCCC1N(CC=CC2=C1C=CC(=C2)OC(N(C)C)=O)C(=O)OC(C)(C)C)(C2=CC=CC=C2)C2=CC=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.8, "product": "C(C)(C)(C)[Si](OCCC1N(CC=CC2=C1C=CC(=C2)OC(N(C)C)=O)C(=O)OC(C)(C)C)(C2=CC=CC=C2)C2=CC=CC=C2", "details": "CALCULATEDPERC...
45
CELSIUS
3
HOUR
To a solution of t-butyl allyl-[3-(t-butyl-diphenyl-silanyloxy)-1-(4-dimethylcarbamoyloxy-2-vinyl-phenyl) -propyl]-carbamate (360 mg, 0.56 mmol) synthesized in step (j) of Example 192 in dichloromethane (40 ml) was added tricyclohexylphosphine [1,3-bis(2,4,6-trimethylphenyl)-4,5-dihydroimidazol-2-ylidene][benzylidene]r...
10.6084/m9.figshare.5104873.v1
null
Allyl.Vinyl
null
null
C1=Cc2ccccc2C[NH]C1
C1=Cc2ccccc2C[NH]C1.c1ccccc1.c1ccccc1
Other
CC1=CC(=C(C(=C1)C)N2CCN([CH-]2)C3=C(C=C(C=C3C)C)C)C.C1CCC(CC1)[PH+](C2CCCCC2)C3CCCCC3.C1=CC=C(C=C1)C=[Ru](Cl)Cl.ClCCl
45
3
C=CCN(C(=O)OC(C)(C)C)C(CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C)c1ccc(OC(=O)N(C)C)cc1C=C>CC1=CC(=C(C(=C1)C)N2CCN([CH-]2)C3=C(C=C(C=C3C)C)C)C.C1CCC(CC1)[PH+](C2CCCCC2)C3CCCCC3.C1=CC=C(C=C1)C=[Ru](Cl)Cl.ClCCl>CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-372570775d5042a6837ac6872a7b4d7e
CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C>>CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO
O.C(C)(C)(C)[Si](OCCC1N(CC=CC2=C1C=CC(=C2)OC(N(C)C)=O)C(=O)OC(C)(C)C)(C2=CC=CC=C2)C2=CC=CC=C2.[F-].C(CCC)[N+](CCCC)(CCCC)CCCC>>CN(C(=O)OC1=CC2=C(C(N(CC=C2)C(=O)OC(C)(C)C)CCO)C=C1)C
CC(C)(C)[Si](c1ccccc1)(c1ccccc1)[O:27][CH2:26][CH2:25][CH:24]1[c:10]2[cH:9][cH:8][c:7]([O:6][C:4]([N:2]([CH3:1])[CH3:3])=[O:5])[cH:12][c:11]2[CH:13]=[CH:14][CH2:15][N:16]1[C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23]>>[CH3:1][N:2]([CH3:3])[C:4](=[O:5])[O:6][c:7]1[cH:8][cH:9][c:10]2[c:11]([cH:12]1)[CH:13]=[CH:...
CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO
null
null
O1CCCC1
Deprotection
Alcohol deprotection from silyl ethers
5607047bc82bb27c5a65769b01ea0774767f4428c871f65da0b6352111d7a6e9
5c02ee98cb6b210a313993bea9e102110eb73637a50746f5457590f98613069b
C1=Cc2ccccc2CNC1
C-C(-C)(-C)-[Si](-[O;H0;D2;+0:1]-[C:2]-[C:3])(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1>>[C:3]-[C:2]-[OH;D1;+0:1]
96
[{"value": 96.0, "product": "CN(C(=O)OC1=CC2=C(C(N(CC=C2)C(=O)OC(C)(C)C)CCO)C=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.0, "product": "CN(C(=O)OC1=CC2=C(C(N(CC=C2)C(=O)OC(C)(C)C)CCO)C=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of t-butyl 1-[2-(t-butyl-diphenyl-silanyloxy)-ethyl]-7-dimethylcarbamoyloxy-1,3-dihydro-benzo[c]azepine-2-carboxylate (1.82 g, 2.96 mmol) synthesized in step (k) of Example 192 in tetrahydrofuran (10 ml) was added 1M solution of tetrabutylammonium fluoride in tetrahydrofuran (6.0 ml, 6.0 mmol) at room tem...
10.6084/m9.figshare.5104873.v1
null
Silyl protective group
Primary alcohol
c1ccccc1.c1ccccc1
null
C1=Cc2ccccc2C[NH]C1
Other
O1CCCC1
null
1
CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C>O1CCCC1>CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9834969e46d8449ab85ba9d5b530563f
CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C>>CN(C)C(=O)Oc1ccc2c(c1)CCCN(C(=O)OC(C)(C)C)C2CCO
C(C)(C)(C)[Si](OCCC1N(CC=CC2=C1C=CC(=C2)OC(N(C)C)=O)C(=O)OC(C)(C)C)(C2=CC=CC=C2)C2=CC=CC=C2>>CN(C(=O)OC1=CC2=C(C(N(CCC2)C(=O)OC(C)(C)C)CCO)C=C1)C
CC(C)(C)[Si](c1ccccc1)(c1ccccc1)[O:27][CH2:26][CH2:25][CH:24]1[c:10]2[cH:9][cH:8][c:7]([O:6][C:4]([N:2]([CH3:1])[CH3:3])=[O:5])[cH:12][c:11]2[CH:13]=[CH:14][CH2:15][N:16]1[C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23]>>[CH3:1][N:2]([CH3:3])[C:4](=[O:5])[O:6][c:7]1[cH:8][cH:9][c:10]2[c:11]([cH:12]1)[CH2:13][CH2...
CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C
CN(C)C(=O)Oc1ccc2c(c1)CCCN(C(=O)OC(C)(C)C)C2CCO
null
[C].[Pd]
CO
Deprotection
OtherReaction
c2fff42fb9a693441092f85389941ed8df04d25c6eaadf1cc5d271208c6c87e1
5c02ee98cb6b210a313993bea9e102110eb73637a50746f5457590f98613069b
c1ccc2c(c1)CCCNC2
C-C(-C)(-C)-[Si](-[O;H0;D2;+0:1]-[C:2]-[C:3]-[C:4]1-[c:5]:[c:6](:[c:7])-[CH;D2;+0:8]=[CH;D2;+0:9]-[C:10]-[#7:11]-1-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15](-[C;D1;H3:16])(-[C;D1;H3:17])-[C;D1;H3:18])(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1>>[C;D1;H3:16]-[C:15](-[C;D1;H3:17])(-[C;D1;H3:18])-[#8:14]-[C:12](=[O;D1;H0:13])-[#7:11]1-[C...
91
[{"value": 91.0, "product": "CN(C(=O)OC1=CC2=C(C(N(CCC2)C(=O)OC(C)(C)C)CCO)C=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.8, "product": "CN(C(=O)OC1=CC2=C(C(N(CCC2)C(=O)OC(C)(C)C)CCO)C=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of t-butyl 7-dimethylcarbamoyloxy-1-(2-hydroxyethyl)-1,3-dihydro-benzo[c]azepine-2-carboxylate (207 mg, 0.550 mmol) synthesized in step (k) of Example 192 in methanol (10 ml) was added 10% palladium carbon (27 mg), and the resulting mixture was stirred for 1 hour at room temperature. After stirring, the r...
10.6084/m9.figshare.5104873.v1
null
Silyl protective group
Primary alcohol
c1ccccc1.c1ccccc1.C1=Cc2ccccc2C[NH]C1
c1ccc2c(c1)CCC[NH]C2
c1ccc2c(c1)CCC[NH]C2
Other
[C].[Pd].CO
null
1
CN(C)C(=O)Oc1ccc2c(c1)C=CCN(C(=O)OC(C)(C)C)C2CCO[Si](c1ccccc1)(c1ccccc1)C(C)(C)C>[C].[Pd].CO>CN(C)C(=O)Oc1ccc2c(c1)CCCN(C(=O)OC(C)(C)C)C2CCO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d9cf3740ba6542ebacbe9a0806229494
ClCc1ccccc1.O=Cc1ccc(O)cc1O>>O=Cc1ccc(OCc2ccccc2)cc1O
OC1=C(C=O)C=CC(=C1)O.C(O)([O-])=O.[Na+].[I-].[K+].C(C1=CC=CC=C1)Cl.Cl>>C(C1=CC=CC=C1)OC1=CC(=C(C=O)C=C1)O
Cl[CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1.[O:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([OH:7])[cH:15][c:16]1[OH:17]>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[cH:15][c:16]1[OH:17]
ClCc1ccccc1.O=Cc1ccc(O)cc1O
O=Cc1ccc(OCc2ccccc2)cc1O
null
null
C(C)#N
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccc(COc2ccccc2)cc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[c:3]:[c:2](-[CH2;D2;+0:1]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]):[c:4]
56
[{"value": 56.0, "product": "C(C1=CC=CC=C1)OC1=CC(=C(C=O)C=C1)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 2,4-dihydroxybenzaldehyde (50.0 g, 362 mmol) in acetonitrile (350 ml) were added sodium hydrogen carbonate (34.6 g, 412 mmol), potassium iodide (6.0 g, 36 mmol), and benzyl chloride (54.0 ml, 470 mmol), and the resulting mixture was refluxed for 24 hours under a nitrogen atmosphere. At the end of the r...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1.c1ccccc1
HCl
C(C)#N
null
null
ClCc1ccccc1.O=Cc1ccc(O)cc1O>C(C)#N>O=Cc1ccc(OCc2ccccc2)cc1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-92a02f518f58487c809bb5ec8470ed73
COCCl.O=Cc1ccc(OCc2ccccc2)cc1O>>COCOc1cc(OCc2ccccc2)ccc1C=O
O.C(C1=CC=CC=C1)OC1=CC(=C(C=O)C=C1)O.C(C)(C)N(CC)C(C)C.COCCl>>C(C1=CC=CC=C1)OC1=CC(=C(C=O)C=C1)OCOC
Cl[CH2:3][O:2][CH3:1].[OH:4][c:5]1[cH:6][c:7]([O:8][CH2:9][c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)[cH:16][cH:17][c:18]1[CH:19]=[O:20]>>[CH3:1][O:2][CH2:3][O:4][c:5]1[cH:6][c:7]([O:8][CH2:9][c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)[cH:16][cH:17][c:18]1[CH:19]=[O:20]
COCCl.O=Cc1ccc(OCc2ccccc2)cc1O
COCOc1cc(OCc2ccccc2)ccc1C=O
null
null
ClCCl
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
6e90ffbf0683e1a3ee55c5e3ea453aefc5ddd369c0150ed0150f9546d7e47f4f
efd670663709b79afcad1306da9f69b33a0147cfa3639ca4c0b54b35ef4b1852
c1ccc(COc2ccccc2)cc1
Cl-[CH2;D2;+0:1]-[#8:2]-[C;D1;H3:3].[O;D1;H0:4]=[C:5]-[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]>>[C;D1;H3:3]-[#8:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:8]-[c:7](:[c:9]):[c:6]-[C:5]=[O;D1;H0:4]
79
[{"value": 79.0, "product": "C(C1=CC=CC=C1)OC1=CC(=C(C=O)C=C1)OCOC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.7, "product": "C(C1=CC=CC=C1)OC1=CC(=C(C=O)C=C1)OCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 4-benzyloxy-2-hydoxy-benzaldehyde (44.9 g, 197 mmol) synthesized in step (a) of Example 197 in dichloromethane (200 ml) were added diisopropylethylamine (52.0 ml, 300 mmol) and methoxymethyl chloride (20.5 ml, 270 mmol) at 0° C. with stirring, and the resulting mixture was stirred overnight at room tem...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Aromatic alcohol
Ether.Ether
null
null
c1ccccc1.c1ccccc1
HCl
ClCCl
null
null
COCCl.O=Cc1ccc(OCc2ccccc2)cc1O>ClCCl>COCOc1cc(OCc2ccccc2)ccc1C=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-cfa6a4fe33564c42bbb76b0af6ce6fb0
CCOC(=O)CP(=O)(OCC)OCC.COCOc1cc(OCc2ccccc2)ccc1C=O>>CCOC(=O)C=Cc1ccc(OCc2ccccc2)cc1OCOC
[H-].[Na+].C(C1=CC=CC=C1)OC1=CC(=C(C=O)C=C1)OCOC.O.C(C)OP(=O)(OCC)CC(=O)OCC>>C(C1=CC=CC=C1)OC1=CC(=C(C=C1)C=CC(=O)OCC)OCOC
CCOP(=O)(OCC)[CH2:6][C:4]([O:3][CH2:2][CH3:1])=[O:5].O=[CH:7][c:8]1[cH:9][cH:10][c:11]([O:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][cH:19]2)[cH:20][c:21]1[O:22][CH2:23][O:24][CH3:25]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]=[CH:7][c:8]1[cH:9][cH:10][c:11]([O:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][cH:19]2)[c...
CCOC(=O)CP(=O)(OCC)OCC.COCOc1cc(OCc2ccccc2)ccc1C=O
CCOC(=O)C=Cc1ccc(OCc2ccccc2)cc1OCOC
null
null
O1CCCC1
C-C Coupling
Wittig with Phosphonium
a86984aeb4a9963534e0b081b0ecca18455fda1775f36ce168d1ca4cf966df3e
203dd34a20dceaf1737adbf20e01b43c2424e4e4b1722d942d1a796d895396e6
c1ccc(COc2ccccc2)cc1
C-C-O-P(=O)(-O-C-C)-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5].O=[CH;D2;+0:6]-[c:7](:[c:8]):[c:9]>>[C:5]-[#8:4]-[C:2](=[O;D1;H0:3])-[CH;D2;+0:1]=[CH;D2;+0:6]-[c:7](:[c:8]):[c:9]
99.3
[{"value": 99.0, "product": "C(C1=CC=CC=C1)OC1=CC(=C(C=C1)C=CC(=O)OCC)OCOC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.3, "product": "C(C1=CC=CC=C1)OC1=CC(=C(C=C1)C=CC(=O)OCC)OCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a suspension of 55% sodium hydride dispersion in mineral oil (1.57 g, 36.0 mmol) in tetrahydrofuran (100 ml) was added ethyl diethylphosphonoacetate (7.17 g, 32.0 mmol) at 0° C. with stirring, and the resulting mixture was stirred for 30 minutes at 0° C. under a nitrogen atmosphere. Subsequently, a solution of 4-ben...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester
Ester
null
null
c1ccccc1.c1ccccc1
HO-
O1CCCC1
null
null
CCOC(=O)CP(=O)(OCC)OCC.COCOc1cc(OCc2ccccc2)ccc1C=O>O1CCCC1>CCOC(=O)C=Cc1ccc(OCc2ccccc2)cc1OCOC
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2e7032211af346cab28f922d73f11869
CCOC(=O)CC(=O)CCl.Nc1ccccn1>>O=c1cc(CCl)nc2ccccn12
NC1=NC=CC=C1.C(C)OC(CC(=O)CCl)=O>>ClCC=1N=C2N(C(C1)=O)C=CC=C2
CCO[C:2](=[O:1])[CH2:3][C:4](=O)[CH2:5][Cl:6].[NH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][n:13]1>>[O:1]=[c:2]1[cH:3][c:4]([CH2:5][Cl:6])[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]12
CCOC(=O)CC(=O)CCl.Nc1ccccn1
O=c1cc(CCl)nc2ccccn12
null
null
null
Aromatic Heterocycle Formation
OtherReaction
18aaa9c9f1fc97f1276b7f3d8d51ea2f879273fca2a44162cb2a6bbc6598427f
65fdd7798538976255c7563b30d8ae7cc21639206d12c4373c064ac8a6ebaebc
O=c1ccnc2ccccn12
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH2;D2;+0:3]-[C;H0;D3;+0:4](=O)-[C:5]-[Cl;D1;H0:6].[NH2;D1;+0:7]-[c:8](:[c:9]):[n;H0;D2;+0:10]:[c:11]:[c:12]>>[Cl;D1;H0:6]-[C:5]-[c;H0;D3;+0:4]1:[cH;D2;+0:3]:[c;H0;D3;+0:1](=[O;D1;H0:2]):[n;H0;D3;+0:10](:[c:11]:[c:12]):[c:8](:[c:9]):[n;H0;D2;+0:7]:1
99
[{"value": 99.0, "product": "ClCC=1N=C2N(C(C1)=O)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.9, "product": "ClCC=1N=C2N(C(C1)=O)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
120
CELSIUS
null
null
15 g (159.4 mmol) of 2-aminopyridine (10) was combined with approximately 80 g of polyphosphoric acid and heated to 120° C. to allow stirring. To the resulting solution was slowly added 30.5 mL (223.2 mmol) of ethyl-4-chloroacetoacetate and stirred at 120° C. under nitrogen for two hours. The hot reaction mixture was t...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Primary amine
null
c1ccncc1
c1ccn2ccccc2n1
c1ccn2ccccc2n1
HO-
null
120
null
CCOC(=O)CC(=O)CCl.Nc1ccccn1>>O=c1cc(CCl)nc2ccccn12
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ad1e9031b79f410db9c8eca5f1bc3535
O=C1CCC(=O)N1I.O=c1cc(CCl)nc2ccccn12>>O=c1c(I)c(CCl)nc2ccccn12
ClCC=1N=C2N(C(C1)=O)C=CC=C2.IN1C(CCC1=O)=O>>ClCC=1N=C2N(C(C1I)=O)C=CC=C2
O=C1CCC(=O)N1[I:4].[O:1]=[c:2]1[cH:3][c:5]([CH2:6][Cl:7])[n:8][c:9]2[cH:10][cH:11][cH:12][cH:13][n:14]12>>[O:1]=[c:2]1[c:3]([I:4])[c:5]([CH2:6][Cl:7])[n:8][c:9]2[cH:10][cH:11][cH:12][cH:13][n:14]12
O=C1CCC(=O)N1I.O=c1cc(CCl)nc2ccccn12
O=c1c(I)c(CCl)nc2ccccn12
null
null
C(C)#N
Functional Group Interconversion
OtherReaction
1f06dfec407448bf0cc30da2662fcfbc61576861352771e24080279cb02cd786
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
O=c1ccnc2ccccn12
O=C1-C-C-C(=O)-N-1-[I;H0;D1;+0:1].[C:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6](:[c:7]):[c:8](=[O;D1;H0:9]):[cH;D2;+0:10]:1>>[C:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6](:[c:7]):[c:8](=[O;D1;H0:9]):[c;H0;D3;+0:10]:1-[I;H0;D1;+0:1]
83
[{"value": 83.0, "product": "ClCC=1N=C2N(C(C1I)=O)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.6, "product": "ClCC=1N=C2N(C(C1I)=O)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
16
HOUR
A mixture of 21.9 g (112.5 mmol) of the product from Step 1 (11) and 38.9 g (168.8 mmol) of N-iodosuccinimide in 660 mL of acetonitrile was stirred at 80° C. under nitrogen for 16 hours. The reaction mixture was then allowed to cool to ambient temperature and the acetonitrile was removed in vacuo. The resulting solid w...
10.6084/m9.figshare.5104873.v1
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Tertiary amide.Tertiary amide
Aromatic halide
C1CCNC1.c1ccn2ccccc2n1
c1cnc2ccccn2c1
c1cnc2ccccn2c1
HO-
C(C)#N
80
16
O=C1CCC(=O)N1I.O=c1cc(CCl)nc2ccccn12>C(C)#N>O=c1c(I)c(CCl)nc2ccccn12
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2a3d0f6d29274e9ea7dca831a61f173c
CC(=O)[O-].O=c1c(I)c(CCl)nc2ccccn12>>CC(=O)OCc1nc2ccccn2c(=O)c1I
ClCC=1N=C2N(C(C1I)=O)C=CC=C2.C(C)(=O)[O-].[K+].O>>C(C)(=O)OCC=1N=C2N(C(C1I)=O)C=CC=C2
[CH3:1][C:2](=[O:3])[O-:4].Cl[CH2:5][c:6]1[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]2[c:14](=[O:15])[c:16]1[I:17]>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][c:6]1[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]2[c:14](=[O:15])[c:16]1[I:17]
CC(=O)[O-].O=c1c(I)c(CCl)nc2ccccn12
CC(=O)OCc1nc2ccccn2c(=O)c1I
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
c07f6f64ff82321b3607467d1ee707cb9bab7ac0cd7c3098b7f6ee7c8546417e
670c5cfed3b5aa12e0b1c180fc6f2dc23f2114806bdb54cf3b29925a677cc9b5
O=c1ccnc2ccccn12
Cl-[CH2;D2;+0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1.[C;D1;H3:8]-[C:9](-[O-;H0;D1:10])=[O;D1;H0:11]>>[C;D1;H3:8]-[C:9](=[O;D1;H0:11])-[O;H0;D2;+0:10]-[CH2;D2;+0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1
90.4
[{"value": 90.0, "product": "C(C)(=O)OCC=1N=C2N(C(C1I)=O)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.4, "product": "C(C)(=O)OCC=1N=C2N(C(C1I)=O)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
40
CELSIUS
3
HOUR
A mixture of 20.0 g (62.4 mmol) of the product from Step 2 (12) and 9.2 g (93.6 mmol) of potassium acetate in 200 mL DMF was stirred at 40° C. under nitrogen for three hours. The reaction mixture was allowed to cool to ambient temperature and the addition of excess water to the reaction solution caused the product to p...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Ester
null
null
c1cnc2ccccn2c1
Other
CN(C)C=O
40
3
CC(=O)[O-].O=c1c(I)c(CCl)nc2ccccn12>CN(C)C=O>CC(=O)OCc1nc2ccccn2c(=O)c1I
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-465f2de5c44f4eafb490bd0a27c9b5c6
O=c1c(I)c(CO)nc2ccccn12.c1ccc(CB2C3CCCC2CCC3)cc1>>O=c1c(Cc2ccccc2)c(CO)nc2ccccn12
OCC=1N=C2N(C(C1I)=O)C=CC=C2.[O-]P(=O)([O-])[O-].[K+].[K+].[K+].[OH-].[Na+].OO.B1(C2CCCC1CCC2)CC3=CC=CC=C3>>C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)CO
I[c:3]1[c:2](=[O:1])[n:20]2[c:15]([n:14][c:11]1[CH2:12][OH:13])[cH:16][cH:17][cH:18][cH:19]2.C1CC2CCCC(C1)B2[CH2:4][c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1>>[O:1]=[c:2]1[c:3]([CH2:4][c:5]2[cH:6][cH:7][cH:8][cH:9][cH:10]2)[c:11]([CH2:12][OH:13])[n:14][c:15]2[cH:16][cH:17][cH:18][cH:19][n:20]12
O=c1c(I)c(CO)nc2ccccn12.c1ccc(CB2C3CCCC2CCC3)cc1
O=c1c(Cc2ccccc2)c(CO)nc2ccccn12
null
C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C(Cl)Cl.Cl[Pd]Cl.[Fe]
CN(C)C=O.C(C)(=O)OCC
C-C Coupling
OtherReaction
f0be20dcbd3a5b120ffc0bdc604159d6719571a9db2f4d60ae9c44e29a64bcf5
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
O=c1c(Cc2ccccc2)cnc2ccccn12
I-[c;H0;D3;+0:1]1:[c:2](-[C:3]):[#7;a:4]:[c:5]:[#7;a:6](:[c:7]):[c:8]:1=[O;D1;H0:9].[c:10]:[c:11](-[CH2;D2;+0:12]-B1-C2-C-C-C-C-1-C-C-C-2):[c:13]>>[C:3]-[c:2]1:[#7;a:4]:[c:5]:[#7;a:6](:[c:7]):[c:8](=[O;D1;H0:9]):[c;H0;D3;+0:1]:1-[CH2;D2;+0:12]-[c:11](:[c:10]):[c:13]
91
[{"value": 91.0, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)CO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.6, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
12
HOUR
A mixture of 4.0 g (13.24 mmol) of the product from Step 4 (14), 1.0 g (1.32 mmol) of dichloro[1,1′-bis(diphenylphosphino)ferrocene] palladium(II) dichloromethane adduct, and 8.4 g (39.72 mmol) of K3PO4 in 30 mL of DMF was heated to 80° C. To the resulting solution was added dropwise 40 mL (19.9 mmol) of B-Benzyl-9-BBN...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1cnc2ccccn2c1.B1C2CCCC1CCC2
c1cnc2ccccn2c1
c1ccccc1.c1cnc2ccccn2c1
HI.B
C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C(Cl)Cl.Cl[Pd]Cl.[Fe].CN(C)C=O.C(C)(=O)OCC
80
12
O=c1c(I)c(CO)nc2ccccn12.c1ccc(CB2C3CCCC2CCC3)cc1>C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C(Cl)Cl.Cl[Pd]Cl.[Fe].CN(C)C=O.C(C)(=O)OCC>O=c1c(Cc2ccccc2)c(CO)nc2ccccn12
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-528b4a3f707542e9930cb18135cacbc2
O=c1c(Cc2ccccc2)c(CO)nc2ccccn12>>O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1
C(C)N(CC)CC.C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)CO.C(C(=O)Cl)(=O)Cl.CS(=O)C>>C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C=O
[OH:1][CH2:2][c:3]1[n:4][c:5]2[cH:6][cH:7][cH:8][cH:9][n:10]2[c:11](=[O:12])[c:13]1[CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1>>[O:1]=[CH:2][c:3]1[n:4][c:5]2[cH:6][cH:7][cH:8][cH:9][n:10]2[c:11](=[O:12])[c:13]1[CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1
O=c1c(Cc2ccccc2)c(CO)nc2ccccn12
O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1
null
null
ClCCl.O.C(C)(=O)OCC
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
O=c1c(Cc2ccccc2)cnc2ccccn12
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:[c:8]:1>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:[c:8]:1
67
[{"value": 67.0, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 66.3, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
1
HOUR
26.5 mL (53.0 mmol) of oxalyl chloride in 40 mL dichloromethane was cooled to −78° C. To the resulting solution was added a solution of 7.52 mL (105.9 mmol) of DMSO in 24 mL dichloromethane and stirred at −78° C. for one hour. Then was added a solution of 4.7 g (17.65 mmol) of the product from Step 5 (15) in 60 mL dich...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1cnc2ccccn2c1.c1ccccc1
null
ClCCl.O.C(C)(=O)OCC
-78
1
O=c1c(Cc2ccccc2)c(CO)nc2ccccn12>ClCCl.O.C(C)(=O)OCC>O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5b3825057f854ccab44104ace7905bbb
C=[C](C)[Mg][Br].O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1>>C=C(C)C(O)c1nc2ccccn2c(=O)c1Cc1ccccc1
C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C=O.C(=C)(C)[Mg]Br>>C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C(C(=C)C)O
[Br][Mg][C:2](=[CH2:1])[CH3:3].[CH:4](=[O:5])[c:6]1[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]2[c:14](=[O:15])[c:16]1[CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1>>[CH2:1]=[C:2]([CH3:3])[CH:4]([OH:5])[c:6]1[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]2[c:14](=[O:15])[c:16]1[CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:...
C=[C](C)[Mg][Br].O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1
C=C(C)C(O)c1nc2ccccn2c(=O)c1Cc1ccccc1
null
null
C1CCOC1
C-C Coupling
Grignard from aldehyde to alcohol
d22306a6b4853561d9b1af524233a68c51df43b11c29a213ef7bf34e1cbc345b
ade448327e9ff2e4739cb0236a603ed53083987df6f7590d564d9a5dce0bda24
O=c1c(Cc2ccccc2)cnc2ccccn12
[Br]-[Mg]-[C;H0;D3;+0:1](=[C;D1;H2:2])-[C;D1;H3:3].[O;H0;D1;+0:4]=[CH;D2;+0:5]-[c:6]1:[#7;a:7]:[c:8]:[#7;a:9]:[c:10]:[c:11]:1>>[C;D1;H2:2]=[C;H0;D3;+0:1](-[C;D1;H3:3])-[CH;D3;+0:5](-[OH;D1;+0:4])-[c:6]1:[#7;a:7]:[c:8]:[#7;a:9]:[c:10]:[c:11]:1
106
[{"value": 106.0, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C(C(=C)C)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 105.3, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C(C(=C)C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
2
HOUR
A mixture of 500 mg (1.9 mmol) of the product from Step 6 (16) in 15 ml THF was cooled to −78° C. To the resulting solution was added dropwise 7.6 ml (3.8 mmol) of isopropenylmagnesium bromide and stirred at −78° C. for 2 hours. The reaction was quenched with saturated NH4Cl and extracted with ethyl acetate (2×). The c...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Aldehyde.Vinyl
Secondary alcohol.Vinyl
null
null
c1cnc2ccccn2c1.c1ccccc1
Br-.Mg
C1CCOC1
-78
2
C=[C](C)[Mg][Br].O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1>C1CCOC1>C=C(C)C(O)c1nc2ccccn2c(=O)c1Cc1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-abdcff8565974421a008799f7eedc0ca
CC(C)C(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.O=C1NC(=O)c2ccccc21>>CC(C)C(c1nc2n(c(=O)c1Cc1ccccc1)CCCC2)N1C(=O)c2ccccc2C1=O
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(C(C)C)O.CC(C)OC(=O)/N=N/C(=O)OC(C)C.C1(C=2C(C(N1)=O)=CC=CC2)=O>>C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(C(C)C)N2C(C1=CC=CC=C1C2=O)=O
O[CH:4]([CH:2]([CH3:1])[CH3:3])[c:5]1[n:6][c:7]2[n:8]([c:9](=[O:10])[c:11]1[CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[CH2:19][CH2:20][CH2:21][CH2:22]2.[NH:23]1[C:24](=[O:25])[c:26]2[cH:27][cH:28][cH:29][cH:30][c:31]2[C:32]1=[O:33]>>[CH3:1][CH:2]([CH3:3])[CH:4]([c:5]1[n:6][c:7]2[n:8]([c:9](=[O:10])[c:11]1[CH2:...
CC(C)C(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.O=C1NC(=O)c2ccccc21
CC(C)C(c1nc2n(c(=O)c1Cc1ccccc1)CCCC2)N1C(=O)c2ccccc2C1=O
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
Mitsunobu_imide
627f58d0e6226c1dbf2a932ee95739face3ceb0131e12fc74fabc98d7152eb3c
7956e5ca56cf10b6e124d86d58ecab05b08a7230f12df133c0e18930774c5c47
O=C1c2ccccc2C(=O)N1Cc1nc2n(c(=O)c1Cc1ccccc1)CCCC2
O-[CH;D3;+0:1](-[C:2](-[C;D1;H3:3])-[C;D1;H3:4])-[c:5]1:[#7;a:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1.[O;D1;H0:11]=[C:12]1-[NH;D2;+0:13]-[C:14](=[O;D1;H0:15])-[c:16]:[c:17]-1>>[C;D1;H3:3]-[C:2](-[C;D1;H3:4])-[CH;D3;+0:1](-[N;H0;D3;+0:13]1-[C:12](=[O;D1;H0:11])-[c:17]:[c:16]-[C:14]-1=[O;D1;H0:15])-[c:5]1:[#7;a:6]:[c:7]:[#7;a:8...
44
[{"value": 44.0, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(C(C)C)N2C(C1=CC=CC=C1C2=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
A previous batch of the product from Step 8 (18) was combined with the above and 150 mg (0.48 mmol) of this crude material was dissolved in 3 ml of dry tetrahydrofuran then cooled to 0° C. Phthalimide 212 mg (1.4 mmol) was added to the cold solution followed by triphenylphosphine 189 mg (0.72 mmol) then DIAD 140 μl (0....
10.6084/m9.figshare.5104873.v1
null
Unsubstituted dicarboximide.Secondary alcohol
Substituted dicarboximide
c1ccc2c(c1)CNC2
c1ccc2c(c1)C[NH]C2
c1ccccc1.c1cnc2n(c1)CCCC2.c1ccc2c(c1)C[NH]C2
HO-
O1CCCC1
0
null
CC(C)C(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.O=C1NC(=O)c2ccccc21>O1CCCC1>CC(C)C(c1nc2n(c(=O)c1Cc1ccccc1)CCCC2)N1C(=O)c2ccccc2C1=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-052f3e5dd9644c4a82306ccb302e5a38
CC(C)C(c1nc2n(c(=O)c1Cc1ccccc1)CCCC2)N1C(=O)c2ccccc2C1=O>>CC(C)C(N)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(C(C)C)N2C(C1=CC=CC=C1C2=O)=O.NN>>NC(C(C)C)C=1N=C2N(C(C1CC1=CC=CC=C1)=O)CCCC2
O=C1c2ccccc2C(=O)[N:5]1[CH:4]([CH:2]([CH3:1])[CH3:3])[c:6]1[n:7][c:8]2[n:9]([c:10](=[O:11])[c:12]1[CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1)[CH2:20][CH2:21][CH2:22][CH2:23]2>>[CH3:1][CH:2]([CH3:3])[CH:4]([NH2:5])[c:6]1[n:7][c:8]2[n:9]([c:10](=[O:11])[c:12]1[CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1)[...
CC(C)C(c1nc2n(c(=O)c1Cc1ccccc1)CCCC2)N1C(=O)c2ccccc2C1=O
CC(C)C(N)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
null
null
C(C)O
Reduction
Phthalimide deprotection
d9f63cee80ef758bd939ff2a10772447b3092f1576180488281833a98eb1691a
dbfe4201a9328005dfaec4c3f363ddbb4ef3c9b825f648735dc97b2b57396333
O=c1c(Cc2ccccc2)cnc2n1CCCC2
O=C1-[N;H0;D3;+0:1](-[C:2](-[C:3])-[c:4]:[#7;a:5])-C(=O)-c2:c:c:c:c:c:2-1>>[#7;a:5]:[c:4]-[C:2](-[C:3])-[NH2;D1;+0:1]
null
[]
null
null
1
HOUR
The product from Step 9 (19), 95 mg (0.22 mmol) was dissolved in 3 ml of dry ethanol then 50 μl (1.6 mmol) of hydrazine was added and the reaction was left to stir at room temperature for 1 h then heated to 40° C. for 2.5 h. The precipitate was removed by filtration and washed with ethyl acetate and the solvent evapora...
10.6084/m9.figshare.5104873.v1
null
Substituted dicarboximide
Primary amine
c1ccc2c(c1)C[NH]C2
null
c1ccccc1.c1cnc2n(c1)CCCC2
HO-
C(C)O
null
1
CC(C)C(c1nc2n(c(=O)c1Cc1ccccc1)CCCC2)N1C(=O)c2ccccc2C1=O>C(C)O>CC(C)C(N)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-569b44ae1a804b5881ce58036529f28d
Cc1ccc(C(=O)N(CCCN2C(=O)c3ccccc3C2=O)C(c2nc3n(c(=O)c2Cc2ccccc2)CCCC3)C(C)C)cc1>>Cc1ccc(C(=O)N(CCCN)C(c2nc3n(c(=O)c2Cc2ccccc2)CCCC3)C(C)C)cc1
C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(C(C)C)N(C(C2=CC=C(C=C2)C)=O)CCCN2C(C1=CC=CC=C1C2=O)=O.NN.C(=O)(C(F)(F)F)O>>NCCCN(C(C1=CC=C(C=C1)C)=O)C(C(C)C)C=1N=C2N(C(C1CC1=CC=CC=C1)=O)CCCC2
O=C1c2ccccc2C(=O)[N:12]1[CH2:11][CH2:10][CH2:9][N:8]([C:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:36][cH:35]1)=[O:7])[CH:13]([c:14]1[n:15][c:16]2[n:17]([c:18](=[O:19])[c:20]1[CH2:21][c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1)[CH2:28][CH2:29][CH2:30][CH2:31]2)[CH:32]([CH3:33])[CH3:34]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([C:6]...
Cc1ccc(C(=O)N(CCCN2C(=O)c3ccccc3C2=O)C(c2nc3n(c(=O)c2Cc2ccccc2)CCCC3)C(C)C)cc1
Cc1ccc(C(=O)N(CCCN)C(c2nc3n(c(=O)c2Cc2ccccc2)CCCC3)C(C)C)cc1
null
null
C(C)O
Reduction
Phthalimide deprotection
d9f63cee80ef758bd939ff2a10772447b3092f1576180488281833a98eb1691a
dbfe4201a9328005dfaec4c3f363ddbb4ef3c9b825f648735dc97b2b57396333
O=C(NCc1nc2n(c(=O)c1Cc1ccccc1)CCCC2)c1ccccc1
O=C1-[N;H0;D3;+0:1](-[C:2]-[C:3])-C(=O)-c2:c:c:c:c:c:2-1>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
null
null
2
HOUR
The product from Step 12 (22), 50 mg (0.08 mmol) was dissolved in 1 ml of anhydrous ethanol. Hydrazine 18 μl (0.57 mmol) was added and the reaction stirred at room temperature for 2 h. The precipitate was filtered through a PTFE filter and washed with ethyl acetate. The solvent was evaporated and the crude material was...
10.6084/m9.figshare.5104873.v1
null
Substituted dicarboximide
Primary amine
c1ccc2c(c1)C[NH]C2
null
c1ccccc1.c1ccccc1.c1cnc2n(c1)CCCC2
HO-
C(C)O
null
2
Cc1ccc(C(=O)N(CCCN2C(=O)c3ccccc3C2=O)C(c2nc3n(c(=O)c2Cc2ccccc2)CCCC3)C(C)C)cc1>C(C)O>Cc1ccc(C(=O)N(CCCN)C(c2nc3n(c(=O)c2Cc2ccccc2)CCCC3)C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2853ad1b901c40ae80bafeada5c16e43
CCOC(=O)CC(=O)CCl.Nc1ccccn1>>O=c1cc(CCl)nc2ccccn12
NC1=NC=CC=C1.C(C)OC(CC(=O)CCl)=O>>ClCC=1N=C2N(C(C1)=O)C=CC=C2
CCO[C:2](=[O:1])[CH2:3][C:4](=O)[CH2:5][Cl:6].[NH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][n:13]1>>[O:1]=[c:2]1[cH:3][c:4]([CH2:5][Cl:6])[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]12
CCOC(=O)CC(=O)CCl.Nc1ccccn1
O=c1cc(CCl)nc2ccccn12
null
null
null
Aromatic Heterocycle Formation
OtherReaction
18aaa9c9f1fc97f1276b7f3d8d51ea2f879273fca2a44162cb2a6bbc6598427f
65fdd7798538976255c7563b30d8ae7cc21639206d12c4373c064ac8a6ebaebc
O=c1ccnc2ccccn12
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH2;D2;+0:3]-[C;H0;D3;+0:4](=O)-[C:5]-[Cl;D1;H0:6].[NH2;D1;+0:7]-[c:8](:[c:9]):[n;H0;D2;+0:10]:[c:11]:[c:12]>>[Cl;D1;H0:6]-[C:5]-[c;H0;D3;+0:4]1:[cH;D2;+0:3]:[c;H0;D3;+0:1](=[O;D1;H0:2]):[n;H0;D3;+0:10](:[c:11]:[c:12]):[c:8](:[c:9]):[n;H0;D2;+0:7]:1
99
[{"value": 99.0, "product": "ClCC=1N=C2N(C(C1)=O)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.9, "product": "ClCC=1N=C2N(C(C1)=O)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
120
CELSIUS
null
null
15 g (159.4 mmol) of 2-aminopyridine (10) was combined with approximately 80 g of polyphosphoric acid and heated to 120° C. to allow stirring. To the resulting solution was added slowly 30.5 mL (223.2 mmol) of ethyl-4-chloroacetoacetate and stirred at 120° C. under nitrogen for two hours. The hot reaction mixture was t...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Primary amine
null
c1ccncc1
c1ccn2ccccc2n1
c1ccn2ccccc2n1
HO-
null
120
null
CCOC(=O)CC(=O)CCl.Nc1ccccn1>>O=c1cc(CCl)nc2ccccn12
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-1ca7ce72ffee42aaba2034928fa59554
O=C1CCC(=O)N1I.O=c1cc(CCl)nc2ccccn12>>O=c1c(I)c(CCl)nc2ccccn12
ClCC=1N=C2N(C(C1)=O)C=CC=C2.IN1C(CCC1=O)=O>>ClCC=1N=C2N(C(C1I)=O)C=CC=C2
O=C1CCC(=O)N1[I:4].[O:1]=[c:2]1[cH:3][c:5]([CH2:6][Cl:7])[n:8][c:9]2[cH:10][cH:11][cH:12][cH:13][n:14]12>>[O:1]=[c:2]1[c:3]([I:4])[c:5]([CH2:6][Cl:7])[n:8][c:9]2[cH:10][cH:11][cH:12][cH:13][n:14]12
O=C1CCC(=O)N1I.O=c1cc(CCl)nc2ccccn12
O=c1c(I)c(CCl)nc2ccccn12
null
null
C(C)#N
Functional Group Interconversion
OtherReaction
1f06dfec407448bf0cc30da2662fcfbc61576861352771e24080279cb02cd786
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
O=c1ccnc2ccccn12
O=C1-C-C-C(=O)-N-1-[I;H0;D1;+0:1].[C:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6](:[c:7]):[c:8](=[O;D1;H0:9]):[cH;D2;+0:10]:1>>[C:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6](:[c:7]):[c:8](=[O;D1;H0:9]):[c;H0;D3;+0:10]:1-[I;H0;D1;+0:1]
83
[{"value": 83.0, "product": "ClCC=1N=C2N(C(C1I)=O)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.6, "product": "ClCC=1N=C2N(C(C1I)=O)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
16
HOUR
A mixture of 21.9 g (112.5 mmol) of the product from Step 1 (11) and 38.9 g (168.8 mmol) of N-iodosuccinimide in 660 mL of acetonitrile was stirred at 80° C. under nitrogen for 16 hours. The reaction mixture was then allowed to cool to ambient temperature and the acetonitrile was removed in vacuo. The resulting solid w...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
C1CCNC1.c1ccn2ccccc2n1
c1cnc2ccccn2c1
c1cnc2ccccn2c1
HO-
C(C)#N
80
16
O=C1CCC(=O)N1I.O=c1cc(CCl)nc2ccccn12>C(C)#N>O=c1c(I)c(CCl)nc2ccccn12
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-4de979b5d68b48d5b058edca74835037
CC(=O)[O-].O=c1c(I)c(CCl)nc2ccccn12>>CC(=O)OCc1nc2ccccn2c(=O)c1I
ClCC=1N=C2N(C(C1I)=O)C=CC=C2.C(C)(=O)[O-].[K+].O>>C(C)(=O)OCC=1N=C2N(C(C1I)=O)C=CC=C2
[CH3:1][C:2](=[O:3])[O-:4].Cl[CH2:5][c:6]1[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]2[c:14](=[O:15])[c:16]1[I:17]>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][c:6]1[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]2[c:14](=[O:15])[c:16]1[I:17]
CC(=O)[O-].O=c1c(I)c(CCl)nc2ccccn12
CC(=O)OCc1nc2ccccn2c(=O)c1I
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
c07f6f64ff82321b3607467d1ee707cb9bab7ac0cd7c3098b7f6ee7c8546417e
670c5cfed3b5aa12e0b1c180fc6f2dc23f2114806bdb54cf3b29925a677cc9b5
O=c1ccnc2ccccn12
Cl-[CH2;D2;+0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1.[C;D1;H3:8]-[C:9](-[O-;H0;D1:10])=[O;D1;H0:11]>>[C;D1;H3:8]-[C:9](=[O;D1;H0:11])-[O;H0;D2;+0:10]-[CH2;D2;+0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1
90.4
[{"value": 90.0, "product": "C(C)(=O)OCC=1N=C2N(C(C1I)=O)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.4, "product": "C(C)(=O)OCC=1N=C2N(C(C1I)=O)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
40
CELSIUS
3
HOUR
A mixture of 20.0 g (62.4 mmol) of the product from Step 2 (12) and 9.2 g (93.6 mmol) of potassium acetate in 200 mL DMF was stirred at 40° C. under nitrogen for three hours. The reaction mixture was allowed to cool to ambient temperature and the addition of excess water to the reaction solution caused the product to p...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Ester
null
null
c1cnc2ccccn2c1
Other
CN(C)C=O
40
3
CC(=O)[O-].O=c1c(I)c(CCl)nc2ccccn12>CN(C)C=O>CC(=O)OCc1nc2ccccn2c(=O)c1I
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ac6d2b19e39f44a79ff89c98a3a3cf91
O=c1c(I)c(CO)nc2ccccn12.c1ccc(CB2C3CCCC2CCC3)cc1>>O=c1c(Cc2ccccc2)c(CO)nc2ccccn12
OCC=1N=C2N(C(C1I)=O)C=CC=C2.[O-]P(=O)([O-])[O-].[K+].[K+].[K+].[OH-].[Na+].OO.B1(C2CCCC1CCC2)CC3=CC=CC=C3>>C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)CO
I[c:3]1[c:2](=[O:1])[n:20]2[c:15]([n:14][c:11]1[CH2:12][OH:13])[cH:16][cH:17][cH:18][cH:19]2.C1CC2CCCC(C1)B2[CH2:4][c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1>>[O:1]=[c:2]1[c:3]([CH2:4][c:5]2[cH:6][cH:7][cH:8][cH:9][cH:10]2)[c:11]([CH2:12][OH:13])[n:14][c:15]2[cH:16][cH:17][cH:18][cH:19][n:20]12
O=c1c(I)c(CO)nc2ccccn12.c1ccc(CB2C3CCCC2CCC3)cc1
O=c1c(Cc2ccccc2)c(CO)nc2ccccn12
null
C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C(Cl)Cl.Cl[Pd]Cl.[Fe]
CN(C)C=O.C(C)(=O)OCC
C-C Coupling
OtherReaction
f0be20dcbd3a5b120ffc0bdc604159d6719571a9db2f4d60ae9c44e29a64bcf5
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
O=c1c(Cc2ccccc2)cnc2ccccn12
I-[c;H0;D3;+0:1]1:[c:2](-[C:3]):[#7;a:4]:[c:5]:[#7;a:6](:[c:7]):[c:8]:1=[O;D1;H0:9].[c:10]:[c:11](-[CH2;D2;+0:12]-B1-C2-C-C-C-C-1-C-C-C-2):[c:13]>>[C:3]-[c:2]1:[#7;a:4]:[c:5]:[#7;a:6](:[c:7]):[c:8](=[O;D1;H0:9]):[c;H0;D3;+0:1]:1-[CH2;D2;+0:12]-[c:11](:[c:10]):[c:13]
91
[{"value": 91.0, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)CO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.6, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
12
HOUR
A mixture of 4.0 g (13.24 mmol) of the product from Step 4 (14), 1.0 g (1.32 mmol) of dichloro[1,1′-bis(diphenylphosphino)ferrocene] palladium(II) dichloromethane adduct, and 8.4 g (39.72 mmol) of K3PO4 in 30 mL of DMF was heated to 80° C. To the resulting solution was added dropwise 40 mL (19.9 mmol) of B-Benzyl-9-BBN...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1cnc2ccccn2c1.B1C2CCCC1CCC2
c1cnc2ccccn2c1
c1ccccc1.c1cnc2ccccn2c1
HI.B
C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C(Cl)Cl.Cl[Pd]Cl.[Fe].CN(C)C=O.C(C)(=O)OCC
80
12
O=c1c(I)c(CO)nc2ccccn12.c1ccc(CB2C3CCCC2CCC3)cc1>C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C1=CC=C(C=C1)[PH+](C2=CC=CC=C2)[C]3[CH][CH][CH][CH]3.C(Cl)Cl.Cl[Pd]Cl.[Fe].CN(C)C=O.C(C)(=O)OCC>O=c1c(Cc2ccccc2)c(CO)nc2ccccn12
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-0a97bb4ce85649a495a0d4155a9906fc
O=c1c(Cc2ccccc2)c(CO)nc2ccccn12>>O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1
C(C)N(CC)CC.C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)CO.C(C(=O)Cl)(=O)Cl.CS(=O)C>>C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C=O
[OH:1][CH2:2][c:3]1[n:4][c:5]2[cH:6][cH:7][cH:8][cH:9][n:10]2[c:11](=[O:12])[c:13]1[CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1>>[O:1]=[CH:2][c:3]1[n:4][c:5]2[cH:6][cH:7][cH:8][cH:9][n:10]2[c:11](=[O:12])[c:13]1[CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1
O=c1c(Cc2ccccc2)c(CO)nc2ccccn12
O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1
null
null
ClCCl.O.C(C)(=O)OCC
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
O=c1c(Cc2ccccc2)cnc2ccccn12
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:[c:8]:1>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:[c:8]:1
67
[{"value": 67.0, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 66.3, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
1
HOUR
26.5 mL (53.0 mmol) of oxalyl chloride in 40 mL dichloromethane was cooled to −78° C. To the resulting solution was added a solution of 7.52 mL (105.9 mmol) of DMSO in 24 mL dichloromethane and stirred at −78° C. for one hour. Then was added a solution of 4.7 g (17.65 mmol) of product from Step 5 (15) in 60 mL dichloro...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1cnc2ccccn2c1.c1ccccc1
null
ClCCl.O.C(C)(=O)OCC
-78
1
O=c1c(Cc2ccccc2)c(CO)nc2ccccn12>ClCCl.O.C(C)(=O)OCC>O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c8395e7f2660426fb4fea0f25dd79e4e
O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1>>C=CC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)C=CC=C2)C=O.C(=C)[Mg]Br>>C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(C=C)O
[CH:3](=[O:4])[c:5]1[n:6][c:7]2[n:8]([c:9](=[O:10])[c:11]1[CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[cH:19][cH:20][cH:21][cH:22]2>>[CH2:1]=[CH:2][CH:3]([OH:4])[c:5]1[n:6][c:7]2[n:8]([c:9](=[O:10])[c:11]1[CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[CH2:19][CH2:20][CH2:21][CH2:22]2
O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1
C=CC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
null
null
C1CCOC1
Miscellaneous
OtherReaction
21fe27eeafdcabda4c34bca4f02b73f86e41d44a0c003f40b099db641d94d557
1cfdacde78204b273e664dc0eb50ffc4dc70522ea435514fcadd01e492b9b547
O=c1c(Cc2ccccc2)cnc2n1CCCC2
[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3]1:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[cH;D2;+0:7]:[cH;D2;+0:8]:[cH;D2;+0:9]:[#7;a:10]:2:[c:11]:[c:12]:1>>[C;D1;H2:13]=[C:14]-[CH;D3;+0:2](-[OH;D1;+0:1])-[c:3]1:[#7;a:4]:[c:5]2:[#7;a:10](:[c:11]:[c:12]:1)-[CH2;D2;+0:9]-[CH2;D2;+0:8]-[CH2;D2;+0:7]-[CH2;D2;+0:6]-2
104.8
[{"value": 104.8, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(C=C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
3
HOUR
A mixture of 2.5 g (9.5 mmol) of the product from Step 6 (16) in 35 mL THF was cooled to −78° C. To the resulting solution was added dropwise 11.4 mL (11.4 mmol) of vinyl magnesium bromide and stirred at −78° C. for 3 hours. The reaction was quenched with saturated NH4Cl and extracted with ethyl acetate (4×). The combi...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Secondary alcohol.Vinyl
c1cnc2ccccn2c1
c1cnc2n(c1)CCCC2
c1ccccc1.c1cnc2n(c1)CCCC2
Other
C1CCOC1
-78
3
O=Cc1nc2ccccn2c(=O)c1Cc1ccccc1>C1CCOC1>C=CC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b09930744d88424abcededd998256f5f
C=CC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2>>CCC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(C=C)O.[H][H]>>C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(CC)O
[CH2:1]=[CH:2][CH:3]([OH:4])[c:5]1[n:6][c:7]2[n:8]([c:9](=[O:10])[c:11]1[CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[CH2:19][CH2:20][CH2:21][CH2:22]2>>[CH3:1][CH2:2][CH:3]([OH:4])[c:5]1[n:6][c:7]2[n:8]([c:9](=[O:10])[c:11]1[CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[CH2:19][CH2:20][CH2:21][CH2:22]2
C=CC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
CCC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
null
[Pd]
C(C)(=O)OCC
Reduction
Hydrogenation (double to single)
8276b4fb5ddc7d15dec6d92474e91e2dbb2fb8b81e5b5720762e5d89cb27aa69
1ccae9f2e86499601fc3421041ff4588c8e6fd53048e86c3b6ed12ae873609c0
O=c1c(Cc2ccccc2)cnc2n1CCCC2
[#7;a:1]:[c:2]-[C:3](-[O;D1;H1:4])-[CH;D2;+0:5]=[CH2;D1;+0:6]>>[#7;a:1]:[c:2]-[C:3](-[O;D1;H1:4])-[CH2;D2;+0:5]-[CH3;D1;+0:6]
85
[{"value": 85.0, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(CC)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.8, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(CC)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
DAY
A mixture of 0.097 g (0.33 mmol) of the product from Step 7 (23) and 0.02 g of Palladium on activated carbon was stirred in 5 mL of ethyl acetate. The flask was equipped with a balloon containing hydrogen gas and the reaction mixture was stirred at ambient temperature for 3 days. The reaction mixture was then filtered ...
10.6084/m9.figshare.5104873.v1
null
Vinyl
null
null
null
c1ccccc1.c1cnc2n(c1)CCCC2
null
[Pd].C(C)(=O)OCC
null
72
C=CC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2>[Pd].C(C)(=O)OCC>CCC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b32bd64ddf9145fab0ed069dc7d2ce92
CCC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.CS(=O)(=O)Cl>>CCC(OS(C)(=O)=O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(CC)O.C(C)N(CC)CC.CS(=O)(=O)Cl>>CS(=O)(=O)OC(CC)C=1N=C2N(C(C1CC1=CC=CC=C1)=O)CCCC2
[CH3:1][CH2:2][CH:3]([OH:4])[c:9]1[n:10][c:11]2[n:12]([c:13](=[O:14])[c:15]1[CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[CH2:23][CH2:24][CH2:25][CH2:26]2.Cl[S:5]([CH3:6])(=[O:7])=[O:8]>>[CH3:1][CH2:2][CH:3]([O:4][S:5]([CH3:6])(=[O:7])=[O:8])[c:9]1[n:10][c:11]2[n:12]([c:13](=[O:14])[c:15]1[CH2:16][c:17]1[cH:18][...
CCC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.CS(=O)(=O)Cl
CCC(OS(C)(=O)=O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
641955d0081c80f158ce2aacd31873a3f3301c87ca0800cf263e288ba8390217
4f9373df8a11470603daf885a5777cebf95940370e32739263d35df0f171a0dd
O=c1c(Cc2ccccc2)cnc2n1CCCC2
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#7;a:5]:[c:6]-[C:7](-[C:8])-[OH;D1;+0:9]>>[#7;a:5]:[c:6]-[C:7](-[C:8])-[O;H0;D2;+0:9]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
100
[{"value": 100.0, "product": "CS(=O)(=O)OC(CC)C=1N=C2N(C(C1CC1=CC=CC=C1)=O)CCCC2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 100.0, "product": "CS(=O)(=O)OC(CC)C=1N=C2N(C(C1CC1=CC=CC=C1)=O)CCCC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
A mixture of 0.084 g (0.28 mmol) of the product (24) from Step 8 and 0.08 mL (0.56 mmol) of triethylamine in 2.5 mL of anhydrous DCM was cooled to 0° C. Then was added dropwise 0.03 mL (0.34 mmol) of methanesulfonyl chloride and the resulting mixture was allowed to warm to ambient temperature under nitrogen. Excess DCM...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Sulfonyl halide
Mesylate
null
null
c1ccccc1.c1cnc2n(c1)CCCC2
HCl
C(Cl)Cl
0
null
CCC(O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.CS(=O)(=O)Cl>C(Cl)Cl>CCC(OS(C)(=O)=O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-42dac9e0cc2e438baefdc9be2c640253
CC(C)(C)OC(=O)NCCCN.CCC(OS(C)(=O)=O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2>>CCC(NCCCNC(=O)OC(C)(C)C)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.N
CS(=O)(=O)OC(CC)C=1N=C2N(C(C1CC1=CC=CC=C1)=O)CCCC2.NCCCNC(OC(C)(C)C)=O.[I-].[K+].CO>>N.C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(CC)NCCCNC(OC(C)(C)C)=O
[NH2:4][CH2:5][CH2:6][CH2:7][NH:8][C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15].CS(=O)(=O)O[CH:3]([CH2:2][CH3:1])[c:16]1[n:17][c:18]2[n:19]([c:20](=[O:21])[c:22]1[CH2:23][c:24]1[cH:25][cH:26][cH:27][cH:28][cH:29]1)[CH2:30][CH2:31][CH2:32][CH2:33]2>>[CH3:1][CH2:2][CH:3]([NH:4][CH2:5][CH2:6][CH2:7][NH:8][C:9](=[...
CC(C)(C)OC(=O)NCCCN.CCC(OS(C)(=O)=O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2
CCC(NCCCNC(=O)OC(C)(C)C)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.N
null
null
C(Cl)Cl.CN(C)C=O
Heteroatom Alkylation and Arylation
Alkylation of amines
8445343b2fb2fd8a9bc06f8532794f2ba6b99565a6e05a3bb9a4344ce2671186
7e6303acde8be57b43b4c6a673e1c7537b1efde90f08932e09e153dbba53a700
O=c1c(Cc2ccccc2)cnc2n1CCCC2
C-S(=O)(=O)-O-[CH;D3;+0:1](-[C:2]-[C;D1;H3:3])-[c:4]1:[#7;a:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[C:10]-[C:11]-[NH2;D1;+0:12]>>[C:10]-[C:11]-[NH;D2;+0:12]-[CH;D3;+0:1](-[C:2]-[C;D1;H3:3])-[c:4]1:[#7;a:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
28.6
[{"value": 0.1, "product": "N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 15.0, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(CC)NCCCNC(OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 28.6, "product": "C(C1=CC=CC=C1)C1=C(N=C2N(C1=O)CCCC2)C(CC)NCCCNC(OC(C)(C)C)=O", "details...
60
CELSIUS
24
HOUR
A mixture of 0.106 g (0.28 mmol) of the product from Step 9 (25), 0.15 g (0.84 mmol) of tert-butyl 3-aminopropylcarbamate, and 0.005 g (0.03 mmol) of potassium iodide in 5 mL of DMF was stirred at 60° C. under nitrogen for 24 hours. The reaction was quenched with water, extracted with ethyl acetate (4×) and the combine...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Primary amine
Secondary amine
null
null
c1ccccc1.c1cnc2n(c1)CCCC2
HO-
C(Cl)Cl.CN(C)C=O
60
24
CC(C)(C)OC(=O)NCCCN.CCC(OS(C)(=O)=O)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2>C(Cl)Cl.CN(C)C=O>CCC(NCCCNC(=O)OC(C)(C)C)c1nc2n(c(=O)c1Cc1ccccc1)CCCC2.N
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5c7803fc28434ac2bf2d75784aa563f6
CI.N#Cc1ccc(OCc2ccccc2)cc1O>>COc1cc(OCc2ccccc2)ccc1C#N
C(C1=CC=CC=C1)OC1=CC(=C(C#N)C=C1)O.IC.[H-].[Na+]>>C(C1=CC=CC=C1)OC1=CC(=C(C#N)C=C1)OC
I[CH3:1].[OH:2][c:3]1[cH:4][c:5]([O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[cH:14][cH:15][c:16]1[C:17]#[N:18]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[cH:14][cH:15][c:16]1[C:17]#[N:18]
CI.N#Cc1ccc(OCc2ccccc2)cc1O
COc1cc(OCc2ccccc2)ccc1C#N
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
b8b041187bac58376aae824630608e7deb49a01db3d652291f8b379c10d4e434
0f0966e3597a58033417ecee71659f4d0c082f95d46b1e52c95541e6e4a59086
c1ccc(COc2ccccc2)cc1
I-[CH3;D1;+0:1].[OH;D1;+0:2]-[c:3](:[c:4]):[c:5]>>[CH3;D1;+0:1]-[O;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]
null
[]
null
null
30
MINUTE
To a magnetically stirred solution of 4-benzyloxy-2-hydroxybenzonitrile (1-A, WO 00/69841) (7.95 g, 35.3 mmol) and iodomethane (5.43 mL, 87.2 mmol) in DMF (90 mL) cooled to −5° was added all at once sodium hydride (60% dispersion, 2.17 g, 54.2 mmol). The mixture was stirred for 30 min, warmed to room temperature and st...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol
Ether
null
null
c1ccccc1.c1ccccc1
HI
CN(C)C=O
null
0.5
CI.N#Cc1ccc(OCc2ccccc2)cc1O>CN(C)C=O>COc1cc(OCc2ccccc2)ccc1C#N
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-7a8d3389992248d6944aa2c1b72ed972
COc1cc(OCc2ccccc2)ccc1C#N.[N-]=[N+]=[N-]>>COc1cc(OCc2ccccc2)ccc1-c1nn[nH]n1
O.C(C1=CC=CC=C1)OC1=CC(=C(C#N)C=C1)OC.[N-]=[N+]=[N-].[Na+].Cl.C(C)N(CC)CC>>C(C1=CC=CC=C1)OC1=CC(=C(C=C1)C=1N=NNN1)OC
[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[cH:14][cH:15][c:16]1[C:17]#[N:18].[N+:19](=[N-:20])=[N-:21]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[cH:14][cH:15][c:16]1-[c:17]1[n:18][n:19][nH:20][n:21]1
COc1cc(OCc2ccccc2)ccc1C#N.[N-]=[N+]=[N-]
COc1cc(OCc2ccccc2)ccc1-c1nn[nH]n1
null
null
C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
237b84aaa459abf427f233dc6a07a1d9de824f980714e458423189bb68f60f12
d8c808528b7ee68720aaeebd35cb6a2a30e344748d0066102cdae99843b93cf0
c1ccc(COc2ccc(-c3nn[nH]n3)cc2)cc1
[#8:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[C;H0;D2;+0:5]#[N;H0;D1;+0:6]):[c:7]:[c:8].[N-;H0;D1:9]=[N+;H0;D2:10]=[N-;H0;D1:11]>>[#8:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[c;H0;D3;+0:5]1:[n;H0;D2;+0:6]:[n;H0;D2;+0:10]:[nH;D2;+0:9]:[n;H0;D2;+0:11]:1):[c:7]:[c:8]
null
[]
null
null
30
MINUTE
A vigorously stirred suspension of 4-benzyloxy-2-methoxybenzonitrile (1-B) (1.20 g, 5.0 mmol), sodium azide (732 mg, 11.3 mmol), and triethylamine hydrochloride (1.54 g, 11.3 mmol) in toluene (6 mL) was heated at 110° for 48 h. The brown suspension was cooled, water (15 mL) was added, and the mixture stirred for 30 min...
10.6084/m9.figshare.5104873.v1
null
Nitrile
null
null
c1nnn[nH]1
c1ccccc1.c1ccccc1.c1nnn[nH]1
null
C1(=CC=CC=C1)C
null
0.5
COc1cc(OCc2ccccc2)ccc1C#N.[N-]=[N+]=[N-]>C1(=CC=CC=C1)C>COc1cc(OCc2ccccc2)ccc1-c1nn[nH]n1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5ba94315f74a4f3da82902ec1853775e
CCCCCC12CCC(c3nnc(-c4ccc(OCc5ccccc5)cc4OC)n3C)(CC1)CC2>>CCCCCC12CCC(c3nnc(-c4ccc(O)cc4OC)n3C)(CC1)CC2
C(C1=CC=CC=C1)OC1=CC(=C(C=C1)C1=NN=C(N1C)C12CCC(CC1)(CC2)CCCCC)OC>>COC=1C=C(C=CC1C1=NN=C(N1C)C12CCC(CC1)(CC2)CCCCC)O
c1ccc(C[O:18][c:17]2[cH:16][cH:15][c:14](-[c:13]3[n:12][n:11][c:10]([C:9]45[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([CH2:26][CH2:25]4)[CH2:28][CH2:27]5)[n:23]3[CH3:24])[c:20]([O:21][CH3:22])[cH:19]2)cc1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([c:10]3[n:11][n:12][c:13](-[c:14]4[cH:...
CCCCCC12CCC(c3nnc(-c4ccc(OCc5ccccc5)cc4OC)n3C)(CC1)CC2
CCCCCC12CCC(c3nnc(-c4ccc(O)cc4OC)n3C)(CC1)CC2
null
[Pd]
CO
Deprotection
Hydroxyl benzyl deprotection
36869d1fe85185a14d9eb30bf05178c600a9b6eca277ffaf3803578c30e0bf5d
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1ccc(-c2nnc(C34CCC(CC3)CC4)[nH]2)cc1
[c:1]:[c:2](-[O;H0;D2;+0:3]-C-c1:c:c:c:c:c:1):[c:4]>>[OH;D1;+0:3]-[c:2](:[c:1]):[c:4]
null
[]
null
null
null
null
A solution of 3-[4-(benzyloxy)-2-methoxyphenyl]-4-methyl-5-(4-pentylbicyclo[2.2.2]oct-1-yl)-4H-1,2,4-triazole (1-E) (272 mg, 0.572 mmol) in MeOH (8 mL) was hydrogenated for 19 h with 10% Pd/C catalyst (27 mg) at room temperature and atmospheric pressure. The catalyst was filtered and washed with MeOH. The MeOH was remo...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
c1ccccc1
null
c1nc[nH]n1.c1ccccc1.C1CC2CCC1CC2
Other
[Pd].CO
null
null
CCCCCC12CCC(c3nnc(-c4ccc(OCc5ccccc5)cc4OC)n3C)(CC1)CC2>[Pd].CO>CCCCCC12CCC(c3nnc(-c4ccc(O)cc4OC)n3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d4b83e628e09444daa2f0b9b64e2c1d2
CCCCCC12CCC(C(=O)O)(CC1)CC2.C[Si](C)(C)C=[N+]=[N-]>>CCCCCC12CCC(C(=O)OC)(CC1)CC2
C[Si](C)(C)C=[N+]=[N-].C(CCCC)C12CCC(CC1)(CC2)C(=O)O>>C(CCCC)C12CCC(CC1)(CC2)C(=O)OC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([C:10](=[O:11])[OH:12])([CH2:14][CH2:15]1)[CH2:16][CH2:17]2.C[Si](C)(C)[CH:13]=[N+]=[N-]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([C:10](=[O:11])[O:12][CH3:13])([CH2:14][CH2:15]1)[CH2:16][CH2:17]2
CCCCCC12CCC(C(=O)O)(CC1)CC2.C[Si](C)(C)C=[N+]=[N-]
CCCCCC12CCC(C(=O)OC)(CC1)CC2
null
null
CO.C(Cl)Cl
Heteroatom Alkylation and Arylation
O-alkylation of carboxylic acids with diazo compounds
39589be0e9a30df66714fe618d22a8ac0fb24901dbf2ead1ab33e31556c7ac64
8b539baf7aeb5ab868833e33306bad77200a853d562904197e13de2e27e229d7
C1CC2CCC1CC2
C-[Si](-C)(-C)-[CH;D2;+0:1]=[N+]=[N-].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
null
[]
null
null
10
MINUTE
(Trimethylsilyl)diazomethane (2M/hexane, 53 mL, 106 mmol) was added slowly to a solution of 4-pentylbicyclo[2.2.2]octane-1-carboxylic acid (2-A) (20.3 g, 90.6 mmol) in methylene chloride (100 mL) and methanol (40 mL) until the yellow color persisted. After stirring for 10 min at room temperature, the solution was conce...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Diazo.Silyl protective group
Ester
null
null
C1CC2CCC1CC2
Other
CO.C(Cl)Cl
null
0.166667
CCCCCC12CCC(C(=O)O)(CC1)CC2.C[Si](C)(C)C=[N+]=[N-]>CO.C(Cl)Cl>CCCCCC12CCC(C(=O)OC)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c6f2bd4daaeb4b90bd37aa6b589eab91
CCCCCC12CCC(C(=O)OC)(CC1)CC2.NN>>CCCCCC12CCC(C(=O)NN)(CC1)CC2
NN.C(CCCC)C12CCC(CC1)(CC2)C(=O)OC.O>>C(CCCC)C12CCC(CC1)(CC2)C(=O)NN
CO[C:10]([C:9]12[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([CH2:15][CH2:14]1)[CH2:17][CH2:16]2)=[O:11].[NH2:12][NH2:13]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([C:10](=[O:11])[NH:12][NH2:13])([CH2:14][CH2:15]1)[CH2:16][CH2:17]2
CCCCCC12CCC(C(=O)OC)(CC1)CC2.NN
CCCCCC12CCC(C(=O)NN)(CC1)CC2
null
null
C(CO)O
Acylation
Aminolysis of esters
2e40a14c7d71c6b9001f460fbb953805c923b2db988c8c04f234b9bb5f04424f
3b636feb164ef0f3c8a4f1764f18a25b9eee32ed1463e3bb4b6f1becb871ca74
C1CC2CCC1CC2
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])(-[C:5])-[C:6].[N;D1;H2:7]-[NH2;D1;+0:8]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:8]-[N;D1;H2:7])(-[C:5])-[C:6]
null
[]
null
null
null
null
Hydrazine (anhydrous, 103 mL, 88.7 mmol) was added to a solution of methyl 4-pentylbicyclo[2.2.2]octane-1-carboxylate (2-B) in ethylene glycol (180 mL) and the mixture was stirred under reflux for 17 h. After cooling to room temperature, the mixture was poured into water (1500 mL) and extracted with methylene chloride ...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ester
Acylhydrazine
null
null
C1CC2CCC1CC2
HO-
C(CO)O
null
null
CCCCCC12CCC(C(=O)OC)(CC1)CC2.NN>C(CO)O>CCCCCC12CCC(C(=O)NN)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d12e7d0d4e094acc9af766b376f160b5
CCCCCC12CCC(C(=O)NN)(CC1)CC2.COc1ccc(C(=O)O)c(C)c1>>CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)o3)(CC1)CC2
C(C)N(CC)CC.[Cl-].ClC=1N(CC[N+]1C)C.CC1=C(C(=O)O)C=CC(=C1)OC.C(CCCC)C12CCC(CC1)(CC2)C(=O)NN>>COC1=CC(=C(C=C1)C=1OC(=NN1)C12CCC(CC1)(CC2)CCCCC)C
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([C:10]([NH:11][NH2:12])=[O:23])([CH2:24][CH2:25]1)[CH2:26][CH2:27]2.O=[C:13](O)[c:14]1[cH:15][cH:16][c:17]([O:18][CH3:19])[cH:20][c:21]1[CH3:22]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([c:10]3[n:11][n:12][c:13](-[c:14]4[cH:15][cH:16][c...
CCCCCC12CCC(C(=O)NN)(CC1)CC2.COc1ccc(C(=O)O)c(C)c1
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)o3)(CC1)CC2
null
null
C(Cl)Cl
Aromatic Heterocycle Formation
OtherReaction
9cd47482aac10ef536f59b494c104bc8c3ef635f3c5e7f741b0b8d333620cea9
6a0a64dedea322c67c78c82295ab9f68e41acfdbf703e197b4f985a15274c989
c1ccc(-c2nnc(C34CCC(CC3)CC4)o2)cc1
O-[C;H0;D3;+0:1](=O)-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5](-[C;D1;H3:6]):[c:7].[C:8]-[C:9](-[C;H0;D3;+0:10](=[O;H0;D1;+0:11])-[NH;D2;+0:12]-[NH2;D1;+0:13])(-[C:14])-[C:15]>>[C:8]-[C:9](-[c;H0;D3;+0:10]1:[n;H0;D2;+0:12]:[n;H0;D2;+0:13]:[c;H0;D3;+0:1](-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5](-[C;D1;H3:6]):[c:7]):[o;H0;D2;+0:11]:...
null
[]
null
null
48
HOUR
2-Chloro-1,3-dimethyl-4,5-dihydro-1H-imidazol-3-ium chloride (5.07 g, 30.0 mmol) was added to a solution of 2-methyl-4-methoxybenzoic acid (2-D) (856 mg, 5.0 mmol) and 4-pentylbicyclo[2.2.2]octane-1-carbohydrazide (2-C) (1.25 g, 5.25 mmol) in methylene chloride (60 mL) followed by triethylamine (8.36 mL, 60 mmol) and t...
10.6084/m9.figshare.5104873.v1
null
Acylhydrazine.Carboxylic acid
null
null
c1nnco1
c1nnco1.c1ccccc1.C1CC2CCC1CC2
HO-
C(Cl)Cl
null
48
CCCCCC12CCC(C(=O)NN)(CC1)CC2.COc1ccc(C(=O)O)c(C)c1>C(Cl)Cl>CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)o3)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e941c7d8cd1b44b5a5fdf3c2ebce4d19
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)o3)(CC1)CC2.CN>>CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)n3C)(CC1)CC2
COC1=CC(=C(C=C1)C=1OC(=NN1)C12CCC(CC1)(CC2)CCCCC)C.FC(C(=O)[O-])(F)F.C[NH3+].CN>>COC1=CC(=C(C=C1)C1=NN=C(N1C)C12CCC(CC1)(CC2)CCCCC)C
o1[c:10]([C:9]23[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([CH2:26][CH2:25]2)[CH2:28][CH2:27]3)[n:11][n:12][c:13]1-[c:14]1[cH:15][cH:16][c:17]([O:18][CH3:19])[cH:20][c:21]1[CH3:22].[NH2:23][CH3:24]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([c:10]3[n:11][n:12][c:13](-[c:14]4[cH:15][cH:...
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)o3)(CC1)CC2.CN
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)n3C)(CC1)CC2
null
null
null
Miscellaneous
OtherReaction
06fefb205a4853de5c4e4a339b564c57a94b95a37d2e8ba13cde385235751498
74f861e099b6420f2f6d4f3094b402eaca1d0baec018283dff42a39bacc23c31
c1ccc(-c2nnc(C34CCC(CC3)CC4)[nH]2)cc1
[C;D1;H3:1]-[NH2;D1;+0:2].[C:3]-[C:4](-[c;H0;D3;+0:5]1:[#7;a:6]:[#7;a:7]:[c;H0;D3;+0:8](-[c:9](:[c:10]):[c:11]):o:1)(-[C:12])-[C:13]>>[C:3]-[C:4](-[c;H0;D3;+0:5]1:[#7;a:6]:[#7;a:7]:[c;H0;D3;+0:8](-[c:9](:[c:10]):[c:11]):[n;H0;D3;+0:2]:1-[C;D1;H3:1])(-[C:12])-[C:13]
null
[]
null
null
null
null
2-(4-Methoxy-2-methylphenyl)-5-(4-pentylbicyclo[2.2.2]oct-1-yl)-1,3,4-oxadiazole (2-E) (988 mg, 2.68 mmol), methylammonium trifluoroacetate (9.72 g, 67 mmol, prepared by combining equimolar amounts of methylamine and trifluoroacetic acid in ether followed by concentration in vacuo), and methylamine (2M/MeOH, 33 mL, 67 ...
10.6084/m9.figshare.5104873.v1
null
Primary amine
null
c1nnco1
c1nc[nH]n1
c1nc[nH]n1.c1ccccc1.C1CC2CCC1CC2
HO-
null
null
null
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)o3)(CC1)CC2.CN>>CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)n3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b1c506f5bd4a4f69afabbbdda5d1ebd2
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)n3C)(CC1)CC2>>CCCCCC12CCC(c3nnc(-c4ccc(O)cc4C)n3C)(CC1)CC2
B(Br)(Br)Br.COC1=CC(=C(C=C1)C1=NN=C(N1C)C12CCC(CC1)(CC2)CCCCC)C>>CC=1C=C(C=CC1C1=NN=C(N1C)C12CCC(CC1)(CC2)CCCCC)O
C[O:18][c:17]1[cH:16][cH:15][c:14](-[c:13]2[n:12][n:11][c:10]([C:9]34[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([CH2:25][CH2:24]3)[CH2:27][CH2:26]4)[n:22]2[CH3:23])[c:20]([CH3:21])[cH:19]1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([c:10]3[n:11][n:12][c:13](-[c:14]4[cH:15][cH:16][c:17]...
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)n3C)(CC1)CC2
CCCCCC12CCC(c3nnc(-c4ccc(O)cc4C)n3C)(CC1)CC2
null
null
C(Cl)Cl
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1ccc(-c2nnc(C34CCC(CC3)CC4)[nH]2)cc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
2
HOUR
Boron tribromide (1M/CH2Cl2, 3.21 mL, 3.21 mmol) was added to a solution of 3-(4-methoxy-2-methylphenyl)4-methyl-5-(4-pentylbicyclo[2.2.2]oct-1-yl)-4H-1,2,4-triazole (2-F) (410 mg, 1.07 mmol) in methylene chloride (6 mL) at 0° C. The mixture was stirred at room temperature for 2 h. The solution was washed with water, 1...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1nc[nH]n1.c1ccccc1.C1CC2CCC1CC2
Other
C(Cl)Cl
null
2
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4C)n3C)(CC1)CC2>C(Cl)Cl>CCCCCC12CCC(c3nnc(-c4ccc(O)cc4C)n3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-592291b2ec824fb19d6e2d104fb4ea04
CCCCCC12CCC(C(=O)O)(CC1)CC2.O=C(Cl)C(=O)Cl>>CCCCCC12CCC(C(=O)Cl)(CC1)CC2
C(C(=O)Cl)(=O)Cl.C(CCCC)C12CCC(CC1)(CC2)C(=O)O>>C(CCCC)C12CCC(CC1)(CC2)C(=O)Cl
O[C:10]([C:9]12[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([CH2:14][CH2:13]1)[CH2:16][CH2:15]2)=[O:11].O=C(Cl)C(=O)[Cl:12]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([C:10](=[O:11])[Cl:12])([CH2:13][CH2:14]1)[CH2:15][CH2:16]2
CCCCCC12CCC(C(=O)O)(CC1)CC2.O=C(Cl)C(=O)Cl
CCCCCC12CCC(C(=O)Cl)(CC1)CC2
null
null
C(Cl)Cl
Functional Group Interconversion
Alcohol to chloride_Other
013cec2edeb273a7a148f349d36a52d99ff4e7bcf8eed78085df830088e387ac
aedb1f68dc5b7eb0583043e1125b741382b17974140a2f46554f0110e2ddc884
C1CC2CCC1CC2
Cl-C(=O)-C(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4](-[C:5])(-[C:6])-[C:7]>>[C:5]-[C:4](-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3])(-[C:6])-[C:7]
null
[]
null
null
3
HOUR
Oxalyl chloride (505 μL, 5.79 mmol) was added dropwise to a mixture of 4-pentylbicyclo[2.2.2]octane-1-carboxylic acid (3-A) in methylene chloride (10 mL). The solution was stirred at room temperature for 3 h and then concentrated in vacuo to give 4-pentylbicyclo[2.2.2]octane-1-carbonyl chloride (3-B). 1H NMR (500 MHz, ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Carboxylic acid
Acyl halide
null
null
C1CC2CCC1CC2
HCl
C(Cl)Cl
null
3
CCCCCC12CCC(C(=O)O)(CC1)CC2.O=C(Cl)C(=O)Cl>C(Cl)Cl>CCCCCC12CCC(C(=O)Cl)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-030e66c4db174e88a95a86231066a60a
CCCCCC12CCC(C(=O)O)(CC1)CC2.CN>>CCCCCC12CCC(C(=O)NC)(CC1)CC2
C(C)(C)N(C(C)C)CC.C(CCCC)C12CCC(CC1)(CC2)C(=O)O.Cl.CN>>CNC(=O)C12CCC(CC1)(CC2)CCCCC
O[C:10]([C:9]12[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([CH2:15][CH2:14]1)[CH2:17][CH2:16]2)=[O:11].[NH2:12][CH3:13]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([C:10](=[O:11])[NH:12][CH3:13])([CH2:14][CH2:15]1)[CH2:16][CH2:17]2
CCCCCC12CCC(C(=O)O)(CC1)CC2.CN
CCCCCC12CCC(C(=O)NC)(CC1)CC2
null
null
C(Cl)Cl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
C1CC2CCC1CC2
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])(-[C:5])-[C:6].[C;D1;H3:7]-[NH2;D1;+0:8]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:8]-[C;D1;H3:7])(-[C:5])-[C:6]
null
[]
null
null
18
HOUR
N,N-Diisopropylethylamine (1.44 mL, 11.1 mmol) was added to a mixture of 4-pentylbicyclo[2.2.2]octane-1-carboxylic acid (3-A) (1.09 g, 4.45 mmol) and methylamine hydrochloride (1.5 g, 22.3 mmol) in methylene chloride (10 mL) was added and the mixture stirred at room temperature for 18 h. After diluting with methylene c...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
C1CC2CCC1CC2
HO-
C(Cl)Cl
null
18
CCCCCC12CCC(C(=O)O)(CC1)CC2.CN>C(Cl)Cl>CCCCCC12CCC(C(=O)NC)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-fbb6f3573a304c5fbaff1f0b87a49bad
CCCCCC12CCC(C(=O)NC)(CC1)CC2.O=C(Cl)C(=O)Cl>>CCCCCC12CCC(C(Cl)=NC)(CC1)CC2
C(C(=O)Cl)(=O)Cl.CNC(=O)C12CCC(CC1)(CC2)CCCCC>>CN=C(C12CCC(CC1)(CC2)CCCCC)Cl
O=[C:10]([C:9]12[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([CH2:15][CH2:14]1)[CH2:17][CH2:16]2)[NH:12][CH3:13].O=C(Cl)C(=O)[Cl:11]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([C:10]([Cl:11])=[N:12][CH3:13])([CH2:14][CH2:15]1)[CH2:16][CH2:17]2
CCCCCC12CCC(C(=O)NC)(CC1)CC2.O=C(Cl)C(=O)Cl
CCCCCC12CCC(C(Cl)=NC)(CC1)CC2
null
null
C(Cl)Cl
Functional Group Interconversion
OtherReaction
dc7791bfee84cf66a1b8f977acbd29af2e1941d3332cba18b7c3de6672d67f79
f77e7aabb720174699de30170bf16b12e447d00eff20d5f78e7a23cf128bc822
C1CC2CCC1CC2
Cl-C(=O)-C(=O)-[Cl;H0;D1;+0:1].O=[C;H0;D3;+0:2](-[NH;D2;+0:3]-[C;D1;H3:4])-[C:5](-[C:6])(-[C:7])-[C:8]>>[C:6]-[C:5](-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[N;H0;D2;+0:3]-[C;D1;H3:4])(-[C:7])-[C:8]
null
[]
null
null
4
HOUR
Oxalyl chloride (846 μL, 9.7 mmol) was added dropwise to a solution of N-methyl-4-pentylbicyclo[2.2.2]octane-1-carboxamide (3-C) (230 mg, 0.97 mmol) in methylene chloride (2.0 mL) and the mixture stirred at room temperature for 4 h. The solvent and excess reagent were removed in vacuo to provide N-methyl-4-pentylbicycl...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Secondary amide
Alkenyl halide
null
null
C1CC2CCC1CC2
HCl
C(Cl)Cl
null
4
CCCCCC12CCC(C(=O)NC)(CC1)CC2.O=C(Cl)C(=O)Cl>C(Cl)Cl>CCCCCC12CCC(C(Cl)=NC)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e64f2088409c4f1e9e76aba2dff66a1b
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4Cl)n3C)(CC1)CC2>>CCCCCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
B(Br)(Br)Br.ClC1=C(C=CC(=C1)OC)C1=NN=C(N1C)C12CCC(CC1)(CC2)CCCCC>>ClC=1C=C(C=CC1C1=NN=C(N1C)C12CCC(CC1)(CC2)CCCCC)O
C[O:18][c:17]1[cH:16][cH:15][c:14](-[c:13]2[n:12][n:11][c:10]([C:9]34[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([CH2:25][CH2:24]3)[CH2:27][CH2:26]4)[n:22]2[CH3:23])[c:20]([Cl:21])[cH:19]1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]12[CH2:7][CH2:8][C:9]([c:10]3[n:11][n:12][c:13](-[c:14]4[cH:15][cH:16][c:17](...
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4Cl)n3C)(CC1)CC2
CCCCCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
null
null
C(Cl)Cl
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1ccc(-c2nnc(C34CCC(CC3)CC4)[nH]2)cc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
2.5
HOUR
Boron tribromide (135 μL, 1.43 mmol) was added dropwise to a solution of 3-(2-chloro-4-methoxyphenyl)-4-methyl-5-(4-pentylbicyclo[2.2.2]oct-1-yl)4H-1,2,4-triazole (3-F) (287 mg, 0.714 mmol) in methylene chloride (5 mL) at 0° C. The mixture was stirred at room temperature for 2.5 h. The solution was washed with water, 1...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1nc[nH]n1.c1ccccc1.C1CC2CCC1CC2
Other
C(Cl)Cl
null
2.5
CCCCCC12CCC(c3nnc(-c4ccc(OC)cc4Cl)n3C)(CC1)CC2>C(Cl)Cl>CCCCCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-bd451761a0974684be9fdb908b83999c
COC(=O)C12CCC(/C=C/CC3(C)OCCO3)(CC1)CC2>>COC(=O)C12CCC(CCCC3(C)OCCO3)(CC1)CC2
CC1(OCCO1)C/C=C/C12CCC(CC1)(CC2)C(=O)OC.[H][H]>>CC1(OCCO1)CCCC12CCC(CC1)(CC2)C(=O)OC
[CH3:1][O:2][C:3](=[O:4])[C:5]12[CH2:6][CH2:7][C:8](/[CH:9]=[CH:10]/[CH2:11][C:12]3([CH3:13])[O:14][CH2:15][CH2:16][O:17]3)([CH2:18][CH2:19]1)[CH2:20][CH2:21]2>>[CH3:1][O:2][C:3](=[O:4])[C:5]12[CH2:6][CH2:7][C:8]([CH2:9][CH2:10][CH2:11][C:12]3([CH3:13])[O:14][CH2:15][CH2:16][O:17]3)([CH2:18][CH2:19]1)[CH2:20][CH2:21]2
COC(=O)C12CCC(/C=C/CC3(C)OCCO3)(CC1)CC2
COC(=O)C12CCC(CCCC3(C)OCCO3)(CC1)CC2
null
[Pd]
C(C)O
Reduction
Hydrogenation (double to single)
0bc3968b35f0839c230afb4215314da278abd4e1f10e42ec3012c5512de49ea5
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
C(CC1OCCO1)CC12CCC(CC1)CC2
[#8:1]-[C:2](-[C:3]/[CH;D2;+0:4]=[CH;D2;+0:5]/[C:6](-[C:7])(-[C:8])-[C:9])-[#8:10]>>[#8:1]-[C:2](-[C:3]-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[C:6](-[C:7])(-[C:8])-[C:9])-[#8:10]
null
[]
null
null
3
HOUR
Methyl 4-[(1E)-3-(2-methyl-1,3-dioxolan-2-yl)prop-1-enyl]bicyclo[2.2.2]octane-1-carboxylate (4-B) (1.1 g) was stirred in ethanol (75 mL). A spatula tip scoop of 10% Pd on carbon (150 mg) was added. A hydrogen balloon was added and the mixture was stirred under hydrogen atmosphere for 3 h. The palladium-on-carbon was fi...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
C1COCO1.C1CC2CCC1CC2
null
[Pd].C(C)O
null
3
COC(=O)C12CCC(/C=C/CC3(C)OCCO3)(CC1)CC2>[Pd].C(C)O>COC(=O)C12CCC(CCCC3(C)OCCO3)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-459c5cfb913d41c4829308c412ec545b
COC(=O)C12CCC(CCCC3(C)OCCO3)(CC1)CC2>>CC1(CCCC23CCC(C(=O)O)(CC2)CC3)OCCO1
Cl.CC1(OCCO1)CCCC12CCC(CC1)(CC2)C(=O)OC.CO.[OH-].[K+]>>CC1(OCCO1)CCCC12CCC(CC1)(CC2)C(=O)O
C[O:12][C:10]([C:9]12[CH2:8][CH2:7][C:6]([CH2:5][CH2:4][CH2:3][C:2]3([CH3:1])[O:17][CH2:18][CH2:19][O:20]3)([CH2:14][CH2:13]1)[CH2:16][CH2:15]2)=[O:11]>>[CH3:1][C:2]1([CH2:3][CH2:4][CH2:5][C:6]23[CH2:7][CH2:8][C:9]([C:10](=[O:11])[OH:12])([CH2:13][CH2:14]2)[CH2:15][CH2:16]3)[O:17][CH2:18][CH2:19][O:20]1
COC(=O)C12CCC(CCCC3(C)OCCO3)(CC1)CC2
CC1(CCCC23CCC(C(=O)O)(CC2)CC3)OCCO1
null
null
O
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
C(CC1OCCO1)CC12CCC(CC1)CC2
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
Methyl 4-[3-(2-methyl-1,3-dioxolan-2-yl)propyl]bicyclo[2.2.2]octane-1-carboxylate (4-C) (1.0 g, 3.38 mmol) was stirred in a solution of 90% methanol and 10% water (50 mL). Excess potassium hydroxide (2.0 g) was added. The mixture was refluxed overnight. The cooled mixture was acidified with 1N hydrochloric acid (100 mL...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1COCO1.C1CC2CCC1CC2
Other
O
null
null
COC(=O)C12CCC(CCCC3(C)OCCO3)(CC1)CC2>O>CC1(CCCC23CCC(C(=O)O)(CC2)CC3)OCCO1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-84fb52185c774a5eb874f0bf0248d023
CC1(CCCC23CCC(c4nnc(-c5ccccc5C(F)(F)F)o4)(CC2)CC3)OCCO1>>CC(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2
CC1(OCCO1)CCCC12CCC(CC1)(CC2)C=2OC(=NN2)C2=C(C=CC=C2)C(F)(F)F.C1(=CC=C(C=C1)S(=O)(=O)O)C>>FC(C1=C(C=CC=C1)C1=NN=C(O1)C12CCC(CC1)(CC2)CCCC(C)=O)(F)F
C1C[O:3][C:2]([CH3:1])([CH2:4][CH2:5][CH2:6][C:7]23[CH2:8][CH2:9][C:10]([c:11]4[n:12][n:13][c:14](-[c:15]5[cH:16][cH:17][cH:18][cH:19][c:20]5[C:21]([F:22])([F:23])[F:24])[o:25]4)([CH2:26][CH2:27]2)[CH2:28][CH2:29]3)O1>>[CH3:1][C:2](=[O:3])[CH2:4][CH2:5][CH2:6][C:7]12[CH2:8][CH2:9][C:10]([c:11]3[n:12][n:13][c:14](-[c:15...
CC1(CCCC23CCC(c4nnc(-c5ccccc5C(F)(F)F)o4)(CC2)CC3)OCCO1
CC(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2
null
null
CC(=O)C
Miscellaneous
Ketal hydrolysis to ketone
bc99a45944d6d67c8bd263755d04463b42623d20ce36570ebfd14e405f44ca50
547697208447432e865290cf95eed8e4fcddc12f59856b7ddbf24dc1accb1210
c1ccc(-c2nnc(C34CCC(CC3)CC4)o2)cc1
[C:1]-[C:2]-[C;H0;D4;+0:3]1(-[C;D1;H3:4])-O-C-C-[O;H0;D2;+0:5]-1>>[C:1]-[C:2]-[C;H0;D3;+0:3](-[C;D1;H3:4])=[O;H0;D1;+0:5]
null
[]
null
null
null
null
2-{4-[3-(2-Methyl-1,3-dioxolan-2-yl)propyl]bicyclo[2.2.2]oct-1-yl}-5-[2-(trifluoromethyl)phenyl]-1,3,4-oxadiazole (4-G) (0.158 g) was stirred in a mixure of 90% acetone/10% water (20 mL). p-Toluenesulfonic acid (10 mg) was added to the solution. The reaction was heated to reflux for 1 h. The volume was reduced by evapo...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Ketone
C1COCO1
null
c1nnco1.c1ccccc1.C1CC2CCC1CC2
HO-
CC(=O)C
null
null
CC1(CCCC23CCC(c4nnc(-c5ccccc5C(F)(F)F)o4)(CC2)CC3)OCCO1>CC(=O)C>CC(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-dbe3666ed85f447b85d247ea660ecf59
CC(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2>>CC(O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2
O.[BH4-].[Na+].FC(C1=C(C=CC=C1)C1=NN=C(O1)C12CCC(CC1)(CC2)CCCC(C)=O)(F)F.C(C)(=O)OCC>>FC(C1=C(C=CC=C1)C1=NN=C(O1)C12CCC(CC1)(CC2)CCCC(C)O)(F)F
[CH3:1][C:2](=[O:3])[CH2:4][CH2:5][CH2:6][C:7]12[CH2:8][CH2:9][C:10]([c:11]3[n:12][n:13][c:14](-[c:15]4[cH:16][cH:17][cH:18][cH:19][c:20]4[C:21]([F:22])([F:23])[F:24])[o:25]3)([CH2:26][CH2:27]1)[CH2:28][CH2:29]2>>[CH3:1][CH:2]([OH:3])[CH2:4][CH2:5][CH2:6][C:7]12[CH2:8][CH2:9][C:10]([c:11]3[n:12][n:13][c:14](-[c:15]4[cH...
CC(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2
CC(O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2
null
null
CO
Reduction
Reduction of ketone to secondary alcohol
02790ac194d8bf7ccb13d6247c59412024d87f77d2c906ef7804f021f57d5070
1bd3cd74b454139c0a0068ac0135836499926b274bff569df163210c6c944a89
c1ccc(-c2nnc(C34CCC(CC3)CC4)o2)cc1
[C:1]-[C:2]-[C;H0;D3;+0:3](-[C;D1;H3:4])=[O;H0;D1;+0:5]>>[C:1]-[C:2]-[CH;D3;+0:3](-[C;D1;H3:4])-[OH;D1;+0:5]
null
[]
null
null
null
null
5-(4-{5-[2-(Trifluoromethyl)phenyl]-1,3,4-oxadiazol-2-yl}bicyclo[2.2.2]oct-1-yl)pentan-2-one (4-H) (0.072 g) was stirred in methanol (2 mL) at 0° C. Sodium borohydride (20 mg) was added. The reaction was allowed to stir to room temperature. The mixture was then layered with ethyl acetate (15 mL) and water (15 mL). The ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
null
null
c1nnco1.c1ccccc1.C1CC2CCC1CC2
null
CO
null
null
CC(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2>CO>CC(O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)o3)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-58f158a836644cc2bae7cfd18667abfe
COc1ccc(-c2nnc(C34CCC(CCCC5(C)OCCO5)(CC3)CC4)o2)c(Cl)c1>>COc1ccc(-c2nnc(C34CCC(CCCC(C)=O)(CC3)CC4)o2)c(Cl)c1
ClC1=C(C=CC(=C1)OC)C=1OC(=NN1)C12CCC(CC1)(CC2)CCCC2(OCCO2)C.C1(=CC=C(C=C1)S(=O)(=O)O)C>>ClC1=C(C=CC(=C1)OC)C1=NN=C(O1)C12CCC(CC1)(CC2)CCCC(C)=O
C1C[O:20][C:18]([CH2:17][CH2:16][CH2:15][C:14]23[CH2:13][CH2:12][C:11]([c:10]4[n:9][n:8][c:7](-[c:6]5[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:28][c:26]5[Cl:27])[o:25]4)([CH2:22][CH2:21]2)[CH2:24][CH2:23]3)([CH3:19])O1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[n:8][n:9][c:10]([C:11]34[CH2:12][CH2:13][C:14]([CH2:15][CH2:16]...
COc1ccc(-c2nnc(C34CCC(CCCC5(C)OCCO5)(CC3)CC4)o2)c(Cl)c1
COc1ccc(-c2nnc(C34CCC(CCCC(C)=O)(CC3)CC4)o2)c(Cl)c1
null
null
CC(=O)C
Miscellaneous
Ketal hydrolysis to ketone
bc99a45944d6d67c8bd263755d04463b42623d20ce36570ebfd14e405f44ca50
547697208447432e865290cf95eed8e4fcddc12f59856b7ddbf24dc1accb1210
c1ccc(-c2nnc(C34CCC(CC3)CC4)o2)cc1
[C:1]-[C:2]-[C;H0;D4;+0:3]1(-[C;D1;H3:4])-O-C-C-[O;H0;D2;+0:5]-1>>[C:1]-[C:2]-[C;H0;D3;+0:3](-[C;D1;H3:4])=[O;H0;D1;+0:5]
null
[]
null
null
null
null
2-(2-Chloro-4-methoxyphenyl)-5-{4-[3-(2-methyl-1,3-dioxolan-2-yl)propyl]bicyclo[2.2.2]oct-1-yl}-1,3,4-oxadiazole (5-G) (0.200 g) was stirred in a mixure of 90% acetone/10% water (20 mL). p-Toluenesulfonic acid (15 mg) was added to the solution. The reaction was heated to reflux for 1 h. The volume was reduced by evapor...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Ketone
C1COCO1
null
c1nnco1.c1ccccc1.C1CC2CCC1CC2
HO-
CC(=O)C
null
null
COc1ccc(-c2nnc(C34CCC(CCCC5(C)OCCO5)(CC3)CC4)o2)c(Cl)c1>CC(=O)C>COc1ccc(-c2nnc(C34CCC(CCCC(C)=O)(CC3)CC4)o2)c(Cl)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d4d247fa61c34f7fb684e5173dbc37e3
COc1ccc(-c2nnc(C34CCC(CCCC(C)=O)(CC3)CC4)o2)c(Cl)c1>>COc1ccc(-c2nnc(C34CCC(CCCC(C)O)(CC3)CC4)o2)c(Cl)c1
O.[BH4-].[Na+].ClC1=C(C=CC(=C1)OC)C1=NN=C(O1)C12CCC(CC1)(CC2)CCCC(C)=O.C(C)(=O)OCC>>ClC1=C(C=CC(=C1)OC)C1=NN=C(O1)C12CCC(CC1)(CC2)CCCC(C)O
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[n:8][n:9][c:10]([C:11]34[CH2:12][CH2:13][C:14]([CH2:15][CH2:16][CH2:17][C:18]([CH3:19])=[O:20])([CH2:21][CH2:22]3)[CH2:23][CH2:24]4)[o:25]2)[c:26]([Cl:27])[cH:28]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[n:8][n:9][c:10]([C:11]34[CH2:12][CH2:13][C:14]([CH2:15][CH2:16][CH2...
COc1ccc(-c2nnc(C34CCC(CCCC(C)=O)(CC3)CC4)o2)c(Cl)c1
COc1ccc(-c2nnc(C34CCC(CCCC(C)O)(CC3)CC4)o2)c(Cl)c1
null
null
CO
Reduction
Reduction of ketone to secondary alcohol
02790ac194d8bf7ccb13d6247c59412024d87f77d2c906ef7804f021f57d5070
1bd3cd74b454139c0a0068ac0135836499926b274bff569df163210c6c944a89
c1ccc(-c2nnc(C34CCC(CC3)CC4)o2)cc1
[C:1]-[C:2]-[C;H0;D3;+0:3](-[C;D1;H3:4])=[O;H0;D1;+0:5]>>[C:1]-[C:2]-[CH;D3;+0:3](-[C;D1;H3:4])-[OH;D1;+0:5]
null
[]
null
null
null
null
5-{4-[5-(2-Chloro-4-methoxyphenyl)-1,3,4-oxadiazol-2-yl]bicyclo[2.2.2]oct-1-yl}pentan-2-one (5-H) (0.150 g, 0.373 mmol) was stirred in methanol (5 mL) at 0° C. Sodium borohydride (0.0169 g, 0.448 mmol) was added. The reaction was allowed to stir to room temperature. The mixture was then layered with ethyl acetate (20 m...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
null
null
c1nnco1.c1ccccc1.C1CC2CCC1CC2
null
CO
null
null
COc1ccc(-c2nnc(C34CCC(CCCC(C)=O)(CC3)CC4)o2)c(Cl)c1>CO>COc1ccc(-c2nnc(C34CCC(CCCC(C)O)(CC3)CC4)o2)c(Cl)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-df60b65268cd4187bb8abcd94d317da8
COc1ccc(-c2nc(C34CCC(CCCC(C)O)(CC3)CC4)nn2C)c(Cl)c1>>CC(O)CCCC12CCC(c3nc(-c4ccc(O)cc4Cl)nn3C)(CC1)CC2
ClC1=C(C=CC(=C1)OC)C1=NC(=NN1C)C12CCC(CC1)(CC2)CCCC(C)O.C(C)[S-].[Na+].C(C)[S-].[Na+]>>ClC=1C=C(C=CC1C1=NN(C(=N1)C12CCC(CC1)(CC2)CCCC(C)O)C)O
C[O:18][c:17]1[cH:16][cH:15][c:14](-[c:13]2[n:12][c:11]([C:10]34[CH2:9][CH2:8][C:7]([CH2:6][CH2:5][CH2:4][CH:2]([CH3:1])[OH:3])([CH2:26][CH2:25]3)[CH2:28][CH2:27]4)[n:23][n:22]2[CH3:24])[c:20]([Cl:21])[cH:19]1>>[CH3:1][CH:2]([OH:3])[CH2:4][CH2:5][CH2:6][C:7]12[CH2:8][CH2:9][C:10]([c:11]3[n:12][c:13](-[c:14]4[cH:15][cH:...
COc1ccc(-c2nc(C34CCC(CCCC(C)O)(CC3)CC4)nn2C)c(Cl)c1
CC(O)CCCC12CCC(c3nc(-c4ccc(O)cc4Cl)nn3C)(CC1)CC2
null
null
CN(C)C=O
Miscellaneous
OtherReaction
af85e5faa5666fd77c1191cff8da8aae98340ec9be0b0764ad456817ff08d81a
0bab01685da92cdead9c84b3a9c513c0e9bd4114585991beae2460d8c47b3623
c1ccc(-c2n[nH]c(C34CCC(CC3)CC4)n2)cc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[c:6]1:[#7;a:7]:[c:8](-[c:9]):[n;H0;D3;+0:10](-[CH3;D1;+0:11]):[n;H0;D2;+0:12]:1>>[C:5]-[c:6]1:[#7;a:7]:[c:8](-[c:9]):[n;H0;D2;+0:10]:[n;H0;D3;+0:12]:1-[CH3;D1;+0:11].[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
5-{4-[5-(2-Chloro-4-methoxyphenyl)-1-methyl-1-H-1,2,4-triazol-3-yl]bicyclo[2.2.2]oct-1-yl}pentan-2-ol (5-J) (0.036 g, 0.086 mmol) was placed in a small vial with 0.5 mL of DMF. Sodium ethanethiolate (0.0218 g, 0.260 mmol) was added to the solution. The vial was sealed and heated to 1000 C for 1.5 h. The incomplete reac...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
c1nnc[nH]1
c1nnc[nH]1
c1nnc[nH]1.c1ccccc1.C1CC2CCC1CC2
Other
CN(C)C=O
null
null
COc1ccc(-c2nc(C34CCC(CCCC(C)O)(CC3)CC4)nn2C)c(Cl)c1>CN(C)C=O>CC(O)CCCC12CCC(c3nc(-c4ccc(O)cc4Cl)nn3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-53742d0c5eb54af9bba80ba6264ee456
CC(O)CCCC12CCC(c3nc(-c4ccc(O)cc4Cl)nn3C)(CC1)CC2>>CC(=O)CCCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
ClC=1C=C(C=CC1C1=NN(C(=N1)C12CCC(CC1)(CC2)CCCC(C)O)C)O.C[N+]1(CCOCC1)[O-]>>ClC1=C(C=CC(=C1)O)C=1N(C(=NN1)C12CCC(CC1)(CC2)CCCC(C)=O)C
[CH3:1][CH:2]([OH:3])[CH2:4][CH2:5][CH2:6][C:7]12[CH2:8][CH2:9][C:10]([c:11]3[n:12]([CH3:24])[n:13][c:14](-[c:15]4[cH:16][cH:17][c:18]([OH:19])[cH:20][c:21]4[Cl:22])[n:23]3)([CH2:25][CH2:26]1)[CH2:27][CH2:28]2>>[CH3:1][C:2](=[O:3])[CH2:4][CH2:5][CH2:6][C:7]12[CH2:8][CH2:9][C:10]([c:11]3[n:12][n:13][c:14](-[c:15]4[cH:16...
CC(O)CCCC12CCC(c3nc(-c4ccc(O)cc4Cl)nn3C)(CC1)CC2
CC(=O)CCCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
null
[Ru](=O)(=O)(=O)[O-].C(CC)[N+](CCC)(CCC)CCC
C(Cl)Cl
Miscellaneous
OtherReaction
5a0da850c5eca3182a8f1192617bc4ffa6221f660a8f48206d6fcbb187f9d1d9
ef59ba7fad669d0d82c4daf03280dc0366c9a31cf6192836b4997e72f66f9d7c
c1ccc(-c2nnc(C34CCC(CC3)CC4)[nH]2)cc1
[C:1]-[C:2]-[CH;D3;+0:3](-[C;D1;H3:4])-[OH;D1;+0:5].[C:6]-[c:7]1:[n;H0;D2;+0:8]:[c:9](-[c:10]):[#7;a:11]:[n;H0;D3;+0:12]:1-[CH3;D1;+0:13]>>[C:1]-[C:2]-[C;H0;D3;+0:3](-[C;D1;H3:4])=[O;H0;D1;+0:5].[C:6]-[c:7]1:[n;H0;D2;+0:12]:[#7;a:11]:[c:9](-[c:10]):[n;H0;D3;+0:8]:1-[CH3;D1;+0:13]
null
[]
null
null
15
MINUTE
3-Chloro-4-{5-[4-(4-hydroxypentyl)bicyclo[2.2.2]oct-1-yl]4-methyl-4H-1,2,4-triazol-3-yl}phenol (5-K) (0.0035 g, 0.00869 mmol) was stirred in 0.5 mL of dry methylene chloride over activated 4 Å sieves. N-methylmorpholine N-oxide (0.0015 g, 0.013 mmol) was added. The mixture was allowed to stir under N2 for 15 min. Tetra...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
c1nc[nH]n1
c1nc[nH]n1
c1nc[nH]n1.c1ccccc1.C1CC2CCC1CC2
null
[Ru](=O)(=O)(=O)[O-].C(CC)[N+](CCC)(CCC)CCC.C(Cl)Cl
null
0.25
CC(O)CCCC12CCC(c3nc(-c4ccc(O)cc4Cl)nn3C)(CC1)CC2>[Ru](=O)(=O)(=O)[O-].C(CC)[N+](CCC)(CCC)CCC.C(Cl)Cl>CC(=O)CCCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-bc0de27bcbc34212928ebda73822b8e1
COC(=O)C12CCC(C(=O)O)(CC1)CC2.NC(=NO)c1ccc(F)cc1>>COC(=O)C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2
COC(=O)C12CCC(CC1)(CC2)C(=O)O.C(=O)(N1C=NC=C1)N1C=NC=C1.FC1=CC=C(C(N)=NO)C=C1>>FC1=CC=C(C=C1)C1=NOC(=N1)C12CCC(CC1)(CC2)C(=O)OC
O=[C:9](O)[C:8]12[CH2:7][CH2:6][C:5]([C:3]([O:2][CH3:1])=[O:4])([CH2:22][CH2:21]1)[CH2:24][CH2:23]2.[NH2:10][C:11]([c:12]1[cH:13][cH:14][c:15]([F:16])[cH:17][cH:18]1)=[N:19][OH:20]>>[CH3:1][O:2][C:3](=[O:4])[C:5]12[CH2:6][CH2:7][C:8]([c:9]3[n:10][c:11](-[c:12]4[cH:13][cH:14][c:15]([F:16])[cH:17][cH:18]4)[n:19][o:20]3)(...
COC(=O)C12CCC(C(=O)O)(CC1)CC2.NC(=NO)c1ccc(F)cc1
COC(=O)C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2
null
null
ClCCl
Aromatic Heterocycle Formation
OtherReaction
a2ae31d0a4419b2c5154a805176ea647c4ecfa171a098253676fdd25dd7bb0eb
125aa09f13da5a63d8a4326b5eb28b82ab752c0f025e52bd5183605dc71565a2
c1ccc(-c2noc(C34CCC(CC3)CC4)n2)cc1
O-[C;H0;D3;+0:1](=O)-[C:2](-[C:3])(-[C:4])-[C:5].[NH2;D1;+0:6]-[C;H0;D3;+0:7](=[N;H0;D2;+0:8]-[OH;D1;+0:9])-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]>>[C:3]-[C:2](-[c;H0;D3;+0:1]1:[n;H0;D2;+0:6]:[c;H0;D3;+0:7](-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]):[n;H0;D2;+0:8]:[o;H0;D2;+0:9]:1)(-[C:4])-[C:5]
null
[]
null
null
1
HOUR
To a suspension of 4-(methoxycarbonyl)bicyclo[2.2.2]octane-1-carboxylic acid (7-A) (0.906 g, 4.27 mmol) in dichloromethane (20 mL) was added 1,1′-carbonyldiimidazole (1.04 g, 6.41 mmol). The reaction turned into a clear solution instantly with evolving of gas. After the mixture was stirred at room temperature for 1 h, ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine.Oxime
null
null
c1ncon1
c1ncon1.c1ccccc1.C1CC2CCC1CC2
HO-
ClCCl
null
1
COC(=O)C12CCC(C(=O)O)(CC1)CC2.NC(=NO)c1ccc(F)cc1>ClCCl>COC(=O)C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-09ebaf0ff92f45e8b1338251305a7176
NNC(=O)c1ccccc1C(F)(F)F.O=C(O)C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2>>Fc1ccc(-c2noc(C34CCC(c5nnc(-c6ccccc6C(F)(F)F)o5)(CC3)CC4)n2)cc1
C(C)N(CC)CC.FC1=CC=C(C=C1)C1=NOC(=N1)C12CCC(CC1)(CC2)C(=O)O.FC(C1=C(C(=O)NN)C=CC=C1)(F)F.[Cl-].ClC1[NH+](CCN1C)C>>FC1=CC=C(C=C1)C1=NOC(=N1)C12CCC(CC1)(CC2)C=2OC(=NN2)C2=C(C=CC=C2)C(F)(F)F
[NH2:15][NH:16][C:17]([c:18]1[cH:19][cH:20][cH:21][cH:22][c:23]1[C:24]([F:25])([F:26])[F:27])=[O:28].O=[C:14](O)[C:13]12[CH2:12][CH2:11][C:10]([c:9]3[o:8][n:7][c:6](-[c:5]4[cH:4][cH:3][c:2]([F:1])[cH:35][cH:34]4)[n:33]3)([CH2:30][CH2:29]1)[CH2:32][CH2:31]2>>[F:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][o:8][c:9]([C:10]34[C...
NNC(=O)c1ccccc1C(F)(F)F.O=C(O)C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2
Fc1ccc(-c2noc(C34CCC(c5nnc(-c6ccccc6C(F)(F)F)o5)(CC3)CC4)n2)cc1
null
null
ClCCl.C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
9cd47482aac10ef536f59b494c104bc8c3ef635f3c5e7f741b0b8d333620cea9
6a0a64dedea322c67c78c82295ab9f68e41acfdbf703e197b4f985a15274c989
c1ccc(-c2noc(C34CCC(c5nnc(-c6ccccc6)o5)(CC3)CC4)n2)cc1
O-[C;H0;D3;+0:1](=O)-[C:2](-[C:3])(-[C:4])-[C:5].[F;D1;H0:6]-[C:7](-[F;D1;H0:8])(-[F;D1;H0:9])-[c:10](:[c:11]):[c;H0;D3;+0:12](-[C;H0;D3;+0:13](=[O;H0;D1;+0:14])-[NH;D2;+0:15]-[NH2;D1;+0:16]):[c:17]:[c:18]>>[C:3]-[C:2](-[c;H0;D3;+0:1]1:[n;H0;D2;+0:16]:[n;H0;D2;+0:15]:[c;H0;D3;+0:13](-[c;H0;D3;+0:12](:[c:17]:[c:18]):[c:...
null
[]
null
null
48
HOUR
A mixture of the acid (7-C) (138.9 mg, 0.439 mmol) and 2-(trifluoromethyl)benzoic hydrazide (7-D) (89.7 mg, 0.439 mmol) was first co-evaporated with toluene three times. Dichloromethane (7 mL) was added to the mixture as solvent. To the resulting suspension was added 2-chloro-1,3-dimethylimidazolinium chloride (743 mg,...
10.6084/m9.figshare.5104873.v1
null
Acylhydrazine.Carboxylic acid
null
null
c1nnco1
c1ncon1.c1nnco1.c1ccccc1.c1ccccc1.C1CC2CCC1CC2
HO-
ClCCl.C1(=CC=CC=C1)C
null
48
NNC(=O)c1ccccc1C(F)(F)F.O=C(O)C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2>ClCCl.C1(=CC=CC=C1)C>Fc1ccc(-c2noc(C34CCC(c5nnc(-c6ccccc6C(F)(F)F)o5)(CC3)CC4)n2)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9ffb1b09c9654cf0ab8b97de94dde1ea
CN.Fc1ccc(-c2noc(C34CCC(c5nnc(-c6ccccc6C(F)(F)F)o5)(CC3)CC4)n2)cc1>>Cn1c(-c2ccccc2C(F)(F)F)nnc1C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2
FC(C(=O)O)(F)F.CN.CN.FC1=CC=C(C=C1)C1=NOC(=N1)C12CCC(CC1)(CC2)C=2OC(=NN2)C2=C(C=CC=C2)C(F)(F)F>>FC1=CC=C(C=C1)C1=NOC(=N1)C12CCC(CC1)(CC2)C2=NN=C(N2C)C2=C(C=CC=C2)C(F)(F)F
[CH3:1][NH2:2].o1[c:3](-[c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[C:10]([F:11])([F:12])[F:13])[n:14][n:15][c:16]1[C:17]12[CH2:18][CH2:19][C:20]([c:21]3[n:22][c:23](-[c:24]4[cH:25][cH:26][c:27]([F:28])[cH:29][cH:30]4)[n:31][o:32]3)([CH2:33][CH2:34]1)[CH2:35][CH2:36]2>>[CH3:1][n:2]1[c:3](-[c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[...
CN.Fc1ccc(-c2noc(C34CCC(c5nnc(-c6ccccc6C(F)(F)F)o5)(CC3)CC4)n2)cc1
Cn1c(-c2ccccc2C(F)(F)F)nnc1C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2
null
null
CO
Miscellaneous
OtherReaction
053ee3bc6819a903779afeaa459454f2cedeb9dc8ad12dec15fa99d829cab5ff
74f861e099b6420f2f6d4f3094b402eaca1d0baec018283dff42a39bacc23c31
c1ccc(-c2noc(C34CCC(c5nnc(-c6ccccc6)[nH]5)(CC3)CC4)n2)cc1
[C;D1;H3:1]-[NH2;D1;+0:2].[C:3]-[C:4](-[c;H0;D3;+0:5]1:[#7;a:6]:[#7;a:7]:[c;H0;D3;+0:8](-[c:9](:[c:10]):[c:11]):o:1)(-[C:12])-[C:13]>>[C:3]-[C:4](-[c;H0;D3;+0:5]1:[#7;a:6]:[#7;a:7]:[c;H0;D3;+0:8](-[c:9](:[c:10]):[c:11]):[n;H0;D3;+0:2]:1-[C;D1;H3:1])(-[C:12])-[C:13]
null
[]
null
null
null
null
A mixture of above 1,2,4-oxadiazole (7-E) (115.2 mg, 0.238 mmol) and the trifluoroacetic acid salt of methylamine (1.73 g, 11.9 mmol) in a 2M solution of methylamine in methanol (4 mL) was heated at 150° C. in a sealed tube for 48 h. The mixture was then concentrated, and the residue was taken up in dichloromethane, wa...
10.6084/m9.figshare.5104873.v1
null
Primary amine
null
c1nnco1
c1nnc[nH]1
c1nnc[nH]1.c1ncon1.c1ccccc1.c1ccccc1.C1CC2CCC1CC2
HO-
CO
null
null
CN.Fc1ccc(-c2noc(C34CCC(c5nnc(-c6ccccc6C(F)(F)F)o5)(CC3)CC4)n2)cc1>CO>Cn1c(-c2ccccc2C(F)(F)F)nnc1C12CCC(c3nc(-c4ccc(F)cc4)no3)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ff54322d153a4dc4b467848c1630342a
NNC(=O)c1ccc(OCc2ccccc2)cc1C(F)(F)F.O=C(O)C12CCC(c3ccccc3)(CC1)CC2>>O=C(NNC(=O)C12CCC(c3ccccc3)(CC1)CC2)c1ccc(OCc2ccccc2)cc1C(F)(F)F
C(C1=CC=CC=C1)OC1=CC(=C(C(=O)NN)C=C1)C(F)(F)F.C1(=CC=CC=C1)C12CCC(CC1)(CC2)C(=O)O.C(C(=O)Cl)(=O)Cl.C(C)N(CC)CC>>C(C1=CC=CC=C1)OC1=CC(=C(C(=O)NNC(=O)C23CCC(CC2)(CC3)C3=CC=CC=C3)C=C1)C(F)(F)F
[O:1]=[C:2]([NH:3][NH2:4])[c:21]1[cH:22][cH:23][c:24]([O:25][CH2:26][c:27]2[cH:28][cH:29][cH:30][cH:31][cH:32]2)[cH:33][c:34]1[C:35]([F:36])([F:37])[F:38].O[C:5](=[O:6])[C:7]12[CH2:8][CH2:9][C:10]([c:11]3[cH:12][cH:13][cH:14][cH:15][cH:16]3)([CH2:17][CH2:18]1)[CH2:19][CH2:20]2>>[O:1]=[C:2]([NH:3][NH:4][C:5](=[O:6])[C:7...
NNC(=O)c1ccc(OCc2ccccc2)cc1C(F)(F)F.O=C(O)C12CCC(c3ccccc3)(CC1)CC2
O=C(NNC(=O)C12CCC(c3ccccc3)(CC1)CC2)c1ccc(OCc2ccccc2)cc1C(F)(F)F
null
CN(C)C=O
C(Cl)Cl
Acylation
Carboxylic acid with primary amine to amide
1bfc5046b360bb38c235d234cdd252f03d34a0792ef57a2cdb032482310d9689
1f93e2b4a6ed796a4645f0486672499ca332a9bc5c180e504c9a46d8eb8d844d
O=C(NNC(=O)C12CCC(c3ccccc3)(CC1)CC2)c1ccc(OCc2ccccc2)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])(-[C:5])-[C:6].[NH2;D1;+0:7]-[#7:8]-[C:9](=[O;D1;H0:10])-[c:11]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:7]-[#7:8]-[C:9](=[O;D1;H0:10])-[c:11])(-[C:5])-[C:6]
null
[]
null
null
30
MINUTE
To a magnetically stirred solution of 4-phenylbicyclo[2.2.2]octane-1-carboxylic acid (8-A) (70 mg, 0.30 mmol) in methylene chloride (1 mL) at room temperature was added 2 M oxalyl chloride in methylene chloride (0.61 mL, 1.22 mmol). Two drops of catalytic DMF were added to catalyze the reaction. The reaction was stirre...
10.6084/m9.figshare.5104873.v1
null
Acylhydrazine.Carboxylic acid
Acylhydrazine.Acylhydrazine
null
null
c1ccccc1.c1ccccc1.c1ccccc1.C1CC2CCC1CC2
HO-
CN(C)C=O.C(Cl)Cl
null
0.5
NNC(=O)c1ccc(OCc2ccccc2)cc1C(F)(F)F.O=C(O)C12CCC(c3ccccc3)(CC1)CC2>CN(C)C=O.C(Cl)Cl>O=C(NNC(=O)C12CCC(c3ccccc3)(CC1)CC2)c1ccc(OCc2ccccc2)cc1C(F)(F)F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8685a6eac8ea44819f3c9fe05917060f
CN.FC(F)(F)c1cc(OCc2ccccc2)ccc1-c1nnc(C23CCC(c4ccccc4)(CC2)CC3)o1>>Cn1c(-c2ccc(OCc3ccccc3)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2
CO.FC(C(=O)[O-])(F)F.CN.CN.C(C1=CC=CC=C1)OC1=CC(=C(C=C1)C=1OC(=NN1)C12CCC(CC1)(CC2)C2=CC=CC=C2)C(F)(F)F>>C(C1=CC=CC=C1)OC1=CC(=C(C=C1)C1=NN=C(N1C)C12CCC(CC1)(CC2)C2=CC=CC=C2)C(F)(F)F
[CH3:1][NH2:2].o1[c:3](-[c:4]2[cH:5][cH:6][c:7]([O:8][CH2:9][c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[cH:16][c:17]2[C:18]([F:19])([F:20])[F:21])[n:22][n:23][c:24]1[C:25]12[CH2:26][CH2:27][C:28]([c:29]3[cH:30][cH:31][cH:32][cH:33][cH:34]3)([CH2:35][CH2:36]1)[CH2:37][CH2:38]2>>[CH3:1][n:2]1[c:3](-[c:4]2[cH:5][cH:6][c:...
CN.FC(F)(F)c1cc(OCc2ccccc2)ccc1-c1nnc(C23CCC(c4ccccc4)(CC2)CC3)o1
Cn1c(-c2ccc(OCc3ccccc3)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2
null
null
null
Miscellaneous
OtherReaction
053ee3bc6819a903779afeaa459454f2cedeb9dc8ad12dec15fa99d829cab5ff
74f861e099b6420f2f6d4f3094b402eaca1d0baec018283dff42a39bacc23c31
c1ccc(COc2ccc(-c3nnc(C45CCC(c6ccccc6)(CC4)CC5)[nH]3)cc2)cc1
[C;D1;H3:1]-[NH2;D1;+0:2].[C:3]-[C:4](-[c;H0;D3;+0:5]1:[#7;a:6]:[#7;a:7]:[c;H0;D3;+0:8](-[c:9](:[c:10]):[c:11]):o:1)(-[C:12])-[C:13]>>[C:3]-[C:4](-[c;H0;D3;+0:5]1:[#7;a:6]:[#7;a:7]:[c;H0;D3;+0:8](-[c:9](:[c:10]):[c:11]):[n;H0;D3;+0:2]:1-[C;D1;H3:1])(-[C:12])-[C:13]
null
[]
150
CELSIUS
null
null
The trifluoroacetate salt of methylamine (380 mg, 2.61 mmol) and 2-[4-(benzyloxy)-2-(trifluoromethyl)phenyl]-5-(4-phenylbicyclo[2.2.2]oct-1-yl)-1,3,4-oxadiazole (8-D) were suspended in a 2 M solution of methylamine in methanol (1.3 mL, 2.61 mmol) and heated at 150° C. overnight. After being-cooled to room temperature, ...
10.6084/m9.figshare.5104873.v1
null
Primary amine
null
c1nnco1
c1nnc[nH]1
c1nnc[nH]1.c1ccccc1.c1ccccc1.c1ccccc1.C1CC2CCC1CC2
HO-
null
150
null
CN.FC(F)(F)c1cc(OCc2ccccc2)ccc1-c1nnc(C23CCC(c4ccccc4)(CC2)CC3)o1>>Cn1c(-c2ccc(OCc3ccccc3)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a0c56182eea249c29f1d65743d49bf35
Cn1c(-c2ccc(OCc3ccccc3)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2>>Cn1c(-c2ccc(O)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2
C(C1=CC=CC=C1)OC1=CC(=C(C=C1)C1=NN=C(N1C)C12CCC(CC1)(CC2)C2=CC=CC=C2)C(F)(F)F>>CN1C(=NN=C1C12CCC(CC1)(CC2)C2=CC=CC=C2)C2=C(C=C(C=C2)O)C(F)(F)F
c1ccc(C[O:8][c:7]2[cH:6][cH:5][c:4](-[c:3]3[n:2]([CH3:1])[c:17]([C:18]45[CH2:19][CH2:20][C:21]([c:22]6[cH:23][cH:24][cH:25][cH:26][cH:27]6)([CH2:28][CH2:29]4)[CH2:30][CH2:31]5)[n:16][n:15]3)[c:10]([C:11]([F:12])([F:13])[F:14])[cH:9]2)cc1>>[CH3:1][n:2]1[c:3](-[c:4]2[cH:5][cH:6][c:7]([OH:8])[cH:9][c:10]2[C:11]([F:12])([F...
Cn1c(-c2ccc(OCc3ccccc3)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2
Cn1c(-c2ccc(O)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2
null
[Pd]
C(C)(=O)OCC.CO
Deprotection
Hydroxyl benzyl deprotection
36869d1fe85185a14d9eb30bf05178c600a9b6eca277ffaf3803578c30e0bf5d
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1ccc(-c2nnc(C34CCC(c5ccccc5)(CC3)CC4)[nH]2)cc1
[c:1]:[c:2](-[O;H0;D2;+0:3]-C-c1:c:c:c:c:c:1):[c:4]>>[OH;D1;+0:3]-[c:2](:[c:1]):[c:4]
null
[]
null
null
3
HOUR
The 3-[4-(Benzyloxy)-2-(trifluoromethyl)phenyl]-4-methyl-5-(4-phenylbicyclo[2.2.2]oct-1-yl)4H-1,2,4-triazole (8-E) (27 mg, 0.05 mmol) was dissolved in ethyl acetate/methanol (1:1, 4 mL) to which 10% palladium-on-carbon (4 mg) was added. The reaction was then placed under hydrogen atmosphere and stirred for 3 h at room ...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
c1ccccc1
null
c1nnc[nH]1.c1ccccc1.c1ccccc1.C1CC2CCC1CC2
Other
[Pd].C(C)(=O)OCC.CO
null
3
Cn1c(-c2ccc(OCc3ccccc3)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2>[Pd].C(C)(=O)OCC.CO>Cn1c(-c2ccc(O)cc2C(F)(F)F)nnc1C12CCC(c3ccccc3)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a286d955ac0a41d1a41f20d217b5c249
CCC12CCC(c3nnc(-c4ccc(OC)cc4Cl)n3C)(CC1)CC2>>CCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
ClC1=C(C=CC(=C1)OC)C1=NN=C(N1C)C12CCC(CC1)(CC2)CC.B(Br)(Br)Br>>ClC=1C=C(C=CC1C1=NN=C(N1C)C12CCC(CC1)(CC2)CC)O
C[O:15][c:14]1[cH:13][cH:12][c:11](-[c:10]2[n:9][n:8][c:7]([C:6]34[CH2:5][CH2:4][C:3]([CH2:2][CH3:1])([CH2:22][CH2:21]3)[CH2:24][CH2:23]4)[n:19]2[CH3:20])[c:17]([Cl:18])[cH:16]1>>[CH3:1][CH2:2][C:3]12[CH2:4][CH2:5][C:6]([c:7]3[n:8][n:9][c:10](-[c:11]4[cH:12][cH:13][c:14]([OH:15])[cH:16][c:17]4[Cl:18])[n:19]3[CH3:20])([...
CCC12CCC(c3nnc(-c4ccc(OC)cc4Cl)n3C)(CC1)CC2
CCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
null
null
C(Cl)Cl
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1ccc(-c2nnc(C34CCC(CC3)CC4)[nH]2)cc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
0
CELSIUS
2
HOUR
Triazole 9-D (30 mg, 0.08 mmol) was dissolved in 0.5 mL of dry methylene chloride, placed under an inert atmosphere, and cooled to 0° C. To this solution was added BBr3 (1 M in CH2Cl2, 0.25 mL, 0.25 mmol) and the cooling bath was immediately removed. The reaction was stirred for 2 h then diluted with 20 mL of methylene...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1nc[nH]n1.c1ccccc1.C1CC2CCC1CC2
Other
C(Cl)Cl
0
2
CCC12CCC(c3nnc(-c4ccc(OC)cc4Cl)n3C)(CC1)CC2>C(Cl)Cl>CCC12CCC(c3nnc(-c4ccc(O)cc4Cl)n3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2c3871ec9b5e41f59191396ebbd8a2c1
CCS(=O)(=O)CCC12CCC(C(=O)OC)(CC1)CC2>>CCS(=O)(=O)CCC12CCC(C(=O)O)(CC1)CC2
C(C)S(=O)(=O)CCC12CCC(CC1)(CC2)C(=O)OC.[OH-].[K+]>>C(C)S(=O)(=O)CCC12CCC(CC1)(CC2)C(=O)O
C[O:14][C:12]([C:11]12[CH2:10][CH2:9][C:8]([CH2:7][CH2:6][S:3]([CH2:2][CH3:1])(=[O:4])=[O:5])([CH2:16][CH2:15]1)[CH2:18][CH2:17]2)=[O:13]>>[CH3:1][CH2:2][S:3](=[O:4])(=[O:5])[CH2:6][CH2:7][C:8]12[CH2:9][CH2:10][C:11]([C:12](=[O:13])[OH:14])([CH2:15][CH2:16]1)[CH2:17][CH2:18]2
CCS(=O)(=O)CCC12CCC(C(=O)OC)(CC1)CC2
CCS(=O)(=O)CCC12CCC(C(=O)O)(CC1)CC2
null
null
O.CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
C1CC2CCC1CC2
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
60
CELSIUS
null
null
Ester 10-3 (880 mg, 3 mmol) was dissolved in 10% water/methanol solution (100 mL) and treated with 1 g of potassium hydroxide. The reaction was heated at 60° C. for 1 h then at 45° C. overnight. The mixture was concentrated in vacuo then acidified to pH 2 with 1M HCl and extracted with three portions of methylene chlor...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CC2CCC1CC2
Other
O.CO
60
null
CCS(=O)(=O)CCC12CCC(C(=O)OC)(CC1)CC2>O.CO>CCS(=O)(=O)CCC12CCC(C(=O)O)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e706c624ca62436c8ab912eeec11dc73
CCS(=O)(=O)CCC12CCC(C(=O)O)(CC1)CC2.CN>>CCS(=O)(=O)CCC12CCC(C(=O)NC)(CC1)CC2
C(C)S(=O)(=O)CCC12CCC(CC1)(CC2)C(=O)O.C(C(=O)Cl)(=O)Cl.CN>>C(C)S(=O)(=O)CCC12CCC(CC1)(CC2)C(=O)NC
O[C:12]([C:11]12[CH2:10][CH2:9][C:8]([CH2:7][CH2:6][S:3]([CH2:2][CH3:1])(=[O:4])=[O:5])([CH2:17][CH2:16]1)[CH2:19][CH2:18]2)=[O:13].[NH2:14][CH3:15]>>[CH3:1][CH2:2][S:3](=[O:4])(=[O:5])[CH2:6][CH2:7][C:8]12[CH2:9][CH2:10][C:11]([C:12](=[O:13])[NH:14][CH3:15])([CH2:16][CH2:17]1)[CH2:18][CH2:19]2
CCS(=O)(=O)CCC12CCC(C(=O)O)(CC1)CC2.CN
CCS(=O)(=O)CCC12CCC(C(=O)NC)(CC1)CC2
null
CN(C)C=O
C(Cl)Cl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
C1CC2CCC1CC2
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])(-[C:5])-[C:6].[C;D1;H3:7]-[NH2;D1;+0:8]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:8]-[C;D1;H3:7])(-[C:5])-[C:6]
null
[]
null
null
90
MINUTE
Carboxylic acid 10-4 (810 mg, 2.96 mmol) was dissolved in 12 mL of anhydrous methylene chloride under nitrogen atmosphere, treated with oxalyl chloride (2M in methylene chloride, 4.4 mL, 8.8 mmol) and subsequently with 5 drops of DMF. The reaction was stirred at room temperature under nitrogen atmosphere for 90 min, th...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
C1CC2CCC1CC2
HO-
CN(C)C=O.C(Cl)Cl
null
1.5
CCS(=O)(=O)CCC12CCC(C(=O)O)(CC1)CC2.CN>CN(C)C=O.C(Cl)Cl>CCS(=O)(=O)CCC12CCC(C(=O)NC)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ef748dab2bdd4380ac279454e952a728
CCS(=O)(=O)CCC12CCC(C(=O)NC)(CC1)CC2.FC(F)(F)c1ccccc1-c1nnn[nH]1>>CCS(=O)(=O)CCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)n3C)(CC1)CC2
C(C)S(=O)(=O)CCC12CCC(CC1)(CC2)C(=O)NC.C(C(=O)Cl)(=O)Cl.FC(C1=C(C=CC=C1)C1=NN=NN1)(F)F>>C(C)S(=O)(=O)CCC12CCC(CC1)(CC2)C2=NN=C(N2C)C2=C(C=CC=C2)C(F)(F)F
O=[C:12]([C:11]12[CH2:10][CH2:9][C:8]([CH2:7][CH2:6][S:3]([CH2:2][CH3:1])(=[O:4])=[O:5])([CH2:29][CH2:28]1)[CH2:31][CH2:30]2)[NH:26][CH3:27].n1[nH][c:15](-[c:16]2[cH:17][cH:18][cH:19][cH:20][c:21]2[C:22]([F:23])([F:24])[F:25])[n:14][n:13]1>>[CH3:1][CH2:2][S:3](=[O:4])(=[O:5])[CH2:6][CH2:7][C:8]12[CH2:9][CH2:10][C:11]([...
CCS(=O)(=O)CCC12CCC(C(=O)NC)(CC1)CC2.FC(F)(F)c1ccccc1-c1nnn[nH]1
CCS(=O)(=O)CCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)n3C)(CC1)CC2
null
CN(C)C=O
C(Cl)Cl
Miscellaneous
OtherReaction
3b312fb2388e7c8a48dfc5e29439e6c80b8d8c210e1557d48baa2e24b968f478
a267a1d067671b1e552868d2a160d189ea3d111697964c07c12357f5fdb70c13
c1ccc(-c2nnc(C34CCC(CC3)CC4)[nH]2)cc1
O=[C;H0;D3;+0:1](-[NH;D2;+0:2]-[C;D1;H3:3])-[C:4](-[C:5])(-[C:6])-[C:7].[c:8]:[c:9](-[c;H0;D3;+0:10]1:[#7;a:11]:[n;H0;D2;+0:12]:n:[nH]:1):[c:13]>>[C:5]-[C:4](-[c;H0;D3;+0:1]1:[n;H0;D2;+0:12]:[#7;a:11]:[c;H0;D3;+0:10](-[c:9](:[c:8]):[c:13]):[n;H0;D3;+0:2]:1-[C;D1;H3:3])(-[C:6])-[C:7]
null
[]
null
null
1
HOUR
Methyl amide 10-5 (220 mg, 0.77 mmol) was dissolved in anhydrous methylene chloride (2 mL) and treated with oxalyl chloride (2M in methylene chloride, 0.77 mL, 1.54 mmol) and DMF (2 drops). The solution was stirred at room temperature for 1 h, then solvent removed by evaporation under diminished pressure. The residue w...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
null
c1nnn[nH]1
c1nc[nH]n1
c1nc[nH]n1.c1ccccc1.C1CC2CCC1CC2
HO-
CN(C)C=O.C(Cl)Cl
null
1
CCS(=O)(=O)CCC12CCC(C(=O)NC)(CC1)CC2.FC(F)(F)c1ccccc1-c1nnn[nH]1>CN(C)C=O.C(Cl)Cl>CCS(=O)(=O)CCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)n3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9d661520c8654c8b94727f04b623984e
COC(=O)C12CCC(/C=C/C(=O)OCc3ccccc3)(CC1)CC2>>COC(=O)C12CCC(CCC(=O)O)(CC1)CC2
C(C)(=O)O.C(C1=CC=CC=C1)OC(/C=C/C12CCC(CC1)(CC2)C(=O)OC)=O>>COC(=O)C12CCC(CC1)(CC2)CCC(=O)O
c1ccc(C[O:13][C:11](/[CH:10]=[CH:9]/[C:8]23[CH2:7][CH2:6][C:5]([C:3]([O:2][CH3:1])=[O:4])([CH2:15][CH2:14]2)[CH2:17][CH2:16]3)=[O:12])cc1>>[CH3:1][O:2][C:3](=[O:4])[C:5]12[CH2:6][CH2:7][C:8]([CH2:9][CH2:10][C:11](=[O:12])[OH:13])([CH2:14][CH2:15]1)[CH2:16][CH2:17]2
COC(=O)C12CCC(/C=C/C(=O)OCc3ccccc3)(CC1)CC2
COC(=O)C12CCC(CCC(=O)O)(CC1)CC2
null
[Pd]
C(C)(=O)OCC.CO
Deprotection
OtherReaction
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
C1CC2CCC1CC2
[C:1]-[C:2](/[CH;D2;+0:3]=[CH;D2;+0:4]/[C:5](=[O;D1;H0:6])-[O;H0;D2;+0:7]-C-c1:c:c:c:c:c:1)(-[C:8])-[C:9]>>[C:1]-[C:2](-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[C:5](=[O;D1;H0:6])-[OH;D1;+0:7])(-[C:8])-[C:9]
null
[]
null
null
2
HOUR
Diester 11-2 (0.625 g, 1.90 mmol) was dissolved in a 1:1 mixture of ethyl acetate/methanol (30 mL), placed under nitrogen atmosphere, then treated with 10% Pd/C (500 mg) and 0.1 mL of acetic acid. The reaction was placed under hydrogen atmosphere and stirred vigorously for 2 hr. The resulting solution was filtered thro...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
C1CC2CCC1CC2
Other
[Pd].C(C)(=O)OCC.CO
null
2
COC(=O)C12CCC(/C=C/C(=O)OCc3ccccc3)(CC1)CC2>[Pd].C(C)(=O)OCC.CO>COC(=O)C12CCC(CCC(=O)O)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9617c9127714410590c90029d8cad091
COC(=O)C12CCC(CCC(=O)O)(CC1)CC2>>COC(=O)C12CCC(CCCO)(CC1)CC2
COC(=O)C12CCC(CC1)(CC2)CCC(=O)O.B.Cl>>OCCCC12CCC(CC1)(CC2)C(=O)OC
O=[C:11]([CH2:10][CH2:9][C:8]12[CH2:7][CH2:6][C:5]([C:3]([O:2][CH3:1])=[O:4])([CH2:14][CH2:13]1)[CH2:16][CH2:15]2)[OH:12]>>[CH3:1][O:2][C:3](=[O:4])[C:5]12[CH2:6][CH2:7][C:8]([CH2:9][CH2:10][CH2:11][OH:12])([CH2:13][CH2:14]1)[CH2:15][CH2:16]2
COC(=O)C12CCC(CCC(=O)O)(CC1)CC2
COC(=O)C12CCC(CCCO)(CC1)CC2
null
null
O1CCCC1
Reduction
Reduction of carboxylic acid to primary alcohol
0db83a5ebe1e318b78b55461cf7eb8f7c004eef0f9e3b6666d3df4c96b5f665e
93b4621647b04d2ad2f2825215b1567f171ba61fe10d136b5db6ea0470aa4932
C1CC2CCC1CC2
O=[C;H0;D3;+0:1](-[O;D1;H1:2])-[C:3]-[C:4]>>[C:4]-[C:3]-[CH2;D2;+0:1]-[O;D1;H1:2]
null
[]
null
null
null
null
Carboxylic acid 11-3 (400 mg, 1.67 mmol) was dissolved in tetrahydrofuran (5 mL) and borane (1 M solution in THF, 2.17 mL, 1.3 eq.) was added dropwise at room temperature. After 2 h the reaction was added to 50 mL of 1 N HCl and then extracted three times with 50 mL of methylene chloride. The combined organic layers we...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary alcohol
null
null
C1CC2CCC1CC2
Other
O1CCCC1
null
null
COC(=O)C12CCC(CCC(=O)O)(CC1)CC2>O1CCCC1>COC(=O)C12CCC(CCCO)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8d49a63409384c689980b386e7f611d6
COC(=O)C12CCC(CCCO)(CC1)CC2.CS(=O)(=O)Cl>>COC(=O)C12CCC(CCCOS(C)(=O)=O)(CC1)CC2
OCCCC12CCC(CC1)(CC2)C(=O)OC.N1=CC=CC=C1.CS(=O)(=O)Cl>>CS(=O)(=O)OCCCC12CCC(CC1)(CC2)C(=O)OC
[CH3:1][O:2][C:3](=[O:4])[C:5]12[CH2:6][CH2:7][C:8]([CH2:9][CH2:10][CH2:11][OH:12])([CH2:17][CH2:18]1)[CH2:19][CH2:20]2.Cl[S:13]([CH3:14])(=[O:15])=[O:16]>>[CH3:1][O:2][C:3](=[O:4])[C:5]12[CH2:6][CH2:7][C:8]([CH2:9][CH2:10][CH2:11][O:12][S:13]([CH3:14])(=[O:15])=[O:16])([CH2:17][CH2:18]1)[CH2:19][CH2:20]2
COC(=O)C12CCC(CCCO)(CC1)CC2.CS(=O)(=O)Cl
COC(=O)C12CCC(CCCOS(C)(=O)=O)(CC1)CC2
null
null
C(Cl)Cl.C(C)(=O)OCC
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
C1CC2CCC1CC2
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6]-[OH;D1;+0:7]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
null
[]
null
null
4
HOUR
Hydroxyester 11-4 (430 mg, 1.9 mmol) was dissolved in 2.5 mL of anhydrous methylene chloride under nitrogen atmosphere, treated with pyridine (0.5 mL) and methanesulfonyl chloride (0.368 mL, 4.8 mmol) and stirred for 4 h at room temperature. The mixture was diluted with 100 mL of ethyl acetate and washed with 1N aqueou...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
C1CC2CCC1CC2
HCl
C(Cl)Cl.C(C)(=O)OCC
null
4
COC(=O)C12CCC(CCCO)(CC1)CC2.CS(=O)(=O)Cl>C(Cl)Cl.C(C)(=O)OCC>COC(=O)C12CCC(CCCOS(C)(=O)=O)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-af2cecdb19664bf285599a4ff49c08f1
CC[S-].COC(=O)C12CCC(CCCOS(C)(=O)=O)(CC1)CC2>>CCSCCCC12CCC(C(=O)OC)(CC1)CC2
CS(=O)(=O)OCCCC12CCC(CC1)(CC2)C(=O)OC.C(C)[S-].[Na+]>>C(C)SCCCC12CCC(CC1)(CC2)C(=O)OC
[CH3:1][CH2:2][S-:3].CS(=O)(=O)O[CH2:4][CH2:5][CH2:6][C:7]12[CH2:8][CH2:9][C:10]([C:11](=[O:12])[O:13][CH3:14])([CH2:15][CH2:16]1)[CH2:17][CH2:18]2>>[CH3:1][CH2:2][S:3][CH2:4][CH2:5][CH2:6][C:7]12[CH2:8][CH2:9][C:10]([C:11](=[O:12])[O:13][CH3:14])([CH2:15][CH2:16]1)[CH2:17][CH2:18]2
CC[S-].COC(=O)C12CCC(CCCOS(C)(=O)=O)(CC1)CC2
CCSCCCC12CCC(C(=O)OC)(CC1)CC2
null
null
CN(C)C=O.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
4ce663f1d715457759f86c3a689fb26031b2c96ac82d1a129bc4ad678e13b486
38c56b8cb3a8c00dfe37ecf8d5a5d7b7efcdb1e68a885b3435776031eb2535b7
C1CC2CCC1CC2
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[C:3].[C;D1;H3:4]-[C:5]-[S-;H0;D1:6]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:6]-[C:5]-[C;D1;H3:4]
null
[]
45
CELSIUS
3
HOUR
Mesylate 11-5 (3.30 g, 10.9 mmol) was dissolved in DMF (20 mL) and treated with sodium ethanethiolate (1.82 g, 21.7 mmol). The solution was stirred at 45° C. for 3 h, then the mixture was diluted with 100 mL of ethyl acetate and washed twice with 1N aqueous HCl, then with saturated aqueous sodium bicarbonate, and brine...
10.6084/m9.figshare.5104873.v1
null
Mesylate
Monosulfide
null
null
C1CC2CCC1CC2
MsOH.HO-
CN(C)C=O.C(C)(=O)OCC
45
3
CC[S-].COC(=O)C12CCC(CCCOS(C)(=O)=O)(CC1)CC2>CN(C)C=O.C(C)(=O)OCC>CCSCCCC12CCC(C(=O)OC)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5ce4bb22dcce4c04888f87d4df956e15
CCS(=O)(=O)CCCC12CCC(C(=O)OC)(CC1)CC2>>CCS(=O)(=O)CCCC12CCC(C(=O)O)(CC1)CC2
C(C)S(=O)(=O)CCCC12CCC(CC1)(CC2)C(=O)OC.[OH-].[K+].Cl>>C(C)S(=O)(=O)CCCC12CCC(CC1)(CC2)C(=O)O
C[O:15][C:13]([C:12]12[CH2:11][CH2:10][C:9]([CH2:8][CH2:7][CH2:6][S:3]([CH2:2][CH3:1])(=[O:4])=[O:5])([CH2:17][CH2:16]1)[CH2:19][CH2:18]2)=[O:14]>>[CH3:1][CH2:2][S:3](=[O:4])(=[O:5])[CH2:6][CH2:7][CH2:8][C:9]12[CH2:10][CH2:11][C:12]([C:13](=[O:14])[OH:15])([CH2:16][CH2:17]1)[CH2:18][CH2:19]2
CCS(=O)(=O)CCCC12CCC(C(=O)OC)(CC1)CC2
CCS(=O)(=O)CCCC12CCC(C(=O)O)(CC1)CC2
null
null
CO.O
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
C1CC2CCC1CC2
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
8
HOUR
Sulfone 11-7 (3.1 g, 10 mmol) was dissolved in 9:1 MeOH/water (50 mL) and treated with potassium hydroxide (3 g). The solution was stirred at room temperature overnight, then the mixture was acidified with 1 N HCl and extracted four times with 50 mL of methylene chloride. The organic layer was dried over anhydrous sodi...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CC2CCC1CC2
Other
CO.O
null
8
CCS(=O)(=O)CCCC12CCC(C(=O)OC)(CC1)CC2>CO.O>CCS(=O)(=O)CCCC12CCC(C(=O)O)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-14428e54e0524b8d822981d4378a9abf
CCS(=O)(=O)CCCC12CCC(C(=O)O)(CC1)CC2.CN>>CCS(=O)(=O)CCCC12CCC(C(=O)NC)(CC1)CC2
CN.C(C)S(=O)(=O)CCCC12CCC(CC1)(CC2)C(=O)O.C(C(=O)Cl)(=O)Cl.CN>>C(C)S(=O)(=O)CCCC12CCC(CC1)(CC2)C(=O)NC
O[C:13]([C:12]12[CH2:11][CH2:10][C:9]([CH2:8][CH2:7][CH2:6][S:3]([CH2:2][CH3:1])(=[O:4])=[O:5])([CH2:18][CH2:17]1)[CH2:20][CH2:19]2)=[O:14].[NH2:15][CH3:16]>>[CH3:1][CH2:2][S:3](=[O:4])(=[O:5])[CH2:6][CH2:7][CH2:8][C:9]12[CH2:10][CH2:11][C:12]([C:13](=[O:14])[NH:15][CH3:16])([CH2:17][CH2:18]1)[CH2:19][CH2:20]2
CCS(=O)(=O)CCCC12CCC(C(=O)O)(CC1)CC2.CN
CCS(=O)(=O)CCCC12CCC(C(=O)NC)(CC1)CC2
null
CN(C)C=O
C(Cl)Cl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
C1CC2CCC1CC2
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])(-[C:5])-[C:6].[C;D1;H3:7]-[NH2;D1;+0:8]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:8]-[C;D1;H3:7])(-[C:5])-[C:6]
null
[]
null
null
90
MINUTE
Carboxylic acid 11-8 (3.0 g, 11 mmol) was dissolved in 50 mL of anhydrous methylene chloride under nitrogen atmosphere, treated with oxalyl chloride (2 M in methylene chloride, 16.2 mL, 32.4 mmol) and subsequently with 5 drops of DMF. The reaction was stirred at room temperature under nitrogen atmosphere for 90 min, th...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
C1CC2CCC1CC2
HO-
CN(C)C=O.C(Cl)Cl
null
1.5
CCS(=O)(=O)CCCC12CCC(C(=O)O)(CC1)CC2.CN>CN(C)C=O.C(Cl)Cl>CCS(=O)(=O)CCCC12CCC(C(=O)NC)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9dbb478b35b94176bb360da1ffb6b9df
CCS(=O)(=O)CCCC12CCC(C(=O)NC)(CC1)CC2.FC(F)(F)c1ccccc1-c1nnn[nH]1>>CCS(=O)(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)n3C)(CC1)CC2
C(C)S(=O)(=O)CCCC12CCC(CC1)(CC2)C(=O)NC.C(C(=O)Cl)(=O)Cl.FC(C1=C(C=CC=C1)C1=NN=NN1)(F)F>>C(C)S(=O)(=O)CCCC12CCC(CC1)(CC2)C2=NN=C(N2C)C2=C(C=CC=C2)C(F)(F)F
O=[C:13]([C:12]12[CH2:11][CH2:10][C:9]([CH2:8][CH2:7][CH2:6][S:3]([CH2:2][CH3:1])(=[O:4])=[O:5])([CH2:30][CH2:29]1)[CH2:32][CH2:31]2)[NH:27][CH3:28].n1[nH][c:16](-[c:17]2[cH:18][cH:19][cH:20][cH:21][c:22]2[C:23]([F:24])([F:25])[F:26])[n:15][n:14]1>>[CH3:1][CH2:2][S:3](=[O:4])(=[O:5])[CH2:6][CH2:7][CH2:8][C:9]12[CH2:10]...
CCS(=O)(=O)CCCC12CCC(C(=O)NC)(CC1)CC2.FC(F)(F)c1ccccc1-c1nnn[nH]1
CCS(=O)(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)n3C)(CC1)CC2
null
CN(C)C=O
C(Cl)Cl
Miscellaneous
OtherReaction
3b312fb2388e7c8a48dfc5e29439e6c80b8d8c210e1557d48baa2e24b968f478
a267a1d067671b1e552868d2a160d189ea3d111697964c07c12357f5fdb70c13
c1ccc(-c2nnc(C34CCC(CC3)CC4)[nH]2)cc1
O=[C;H0;D3;+0:1](-[NH;D2;+0:2]-[C;D1;H3:3])-[C:4](-[C:5])(-[C:6])-[C:7].[c:8]:[c:9](-[c;H0;D3;+0:10]1:[#7;a:11]:[n;H0;D2;+0:12]:n:[nH]:1):[c:13]>>[C:5]-[C:4](-[c;H0;D3;+0:1]1:[n;H0;D2;+0:12]:[#7;a:11]:[c;H0;D3;+0:10](-[c:9](:[c:8]):[c:13]):[n;H0;D3;+0:2]:1-[C;D1;H3:3])(-[C:6])-[C:7]
null
[]
null
null
1
HOUR
Methyl amide 11-9 (0.470 g, 1.56 mmol) was dissolved in anhydrous methylene chloride (5 mL) and treated with oxalyl chloride (2M in methylene chloride, 1.56 mL, 3.12 mmol) and DMF (2 drops). The solution was stirred at room temperature for 1 h, then solvent removed by evaporation under reduced pressure. The residue was...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
null
c1nnn[nH]1
c1nc[nH]n1
c1nc[nH]n1.c1ccccc1.C1CC2CCC1CC2
HO-
CN(C)C=O.C(Cl)Cl
null
1
CCS(=O)(=O)CCCC12CCC(C(=O)NC)(CC1)CC2.FC(F)(F)c1ccccc1-c1nnn[nH]1>CN(C)C=O.C(Cl)Cl>CCS(=O)(=O)CCCC12CCC(c3nnc(-c4ccccc4C(F)(F)F)n3C)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-25cc8f7fb801465897a61ea3c50f29e0
COC(=O)C12CCC(C=O)(CC1)CC2.C[Si](C)(C)[N-][Si](C)(C)C>>C=CC12CCC(C(=O)OC)(CC1)CC2
C(=O)C12CCC(CC1)(CC2)C(=O)OC.C[Si]([N-][Si](C)(C)C)(C)C.[K+]>>C(=C)C12CCC(CC1)(CC2)C(=O)OC
O=[CH:2][C:3]12[CH2:4][CH2:5][C:6]([C:7](=[O:8])[O:9][CH3:10])([CH2:11][CH2:12]1)[CH2:13][CH2:14]2.C[Si](C)(C)[N-][Si](C)(C)[CH3:1]>>[CH2:1]=[CH:2][C:3]12[CH2:4][CH2:5][C:6]([C:7](=[O:8])[O:9][CH3:10])([CH2:11][CH2:12]1)[CH2:13][CH2:14]2
COC(=O)C12CCC(C=O)(CC1)CC2.C[Si](C)(C)[N-][Si](C)(C)C
C=CC12CCC(C(=O)OC)(CC1)CC2
null
[Br-].C[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1
CCOC(=O)C.C1CCOC1
C-C Coupling
OtherReaction
65846b40393caf810f4a2d80980311afbe6a487d5b2731f135215f55a25e4832
37f02ff997533d11a1e569347ef78cf65235ab0024b34a145afdaafd2d3d15ac
C1CC2CCC1CC2
C-[Si](-C)(-C)-[N-]-[Si](-C)(-C)-[CH3;D1;+0:1].O=[CH;D2;+0:2]-[C:3](-[C:4])(-[C:5])-[C:6]>>[C:4]-[C:3](-[CH;D2;+0:2]=[CH2;D1;+0:1])(-[C:5])-[C:6]
null
[]
null
null
5
MINUTE
To a stirred solution of methyltriphenylphosphonium bromide (9.1 g, 12.8 mmol) in THF (50 ml) at 0° C. was added potassium hexamethyldisilazide (0.5M in toluene, 48.6 ml), dropwise over 5 min. The resulting mixture was allowed to warm up to room temperature over 1 h, then cooled again to 0° C. and treated with methyl 4...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Silyl protective group.Silyl protective group
Vinyl
null
null
C1CC2CCC1CC2
HO-
[Br-].C[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.CCOC(=O)C.C1CCOC1
null
0.083333
COC(=O)C12CCC(C=O)(CC1)CC2.C[Si](C)(C)[N-][Si](C)(C)C>[Br-].C[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.CCOC(=O)C.C1CCOC1>C=CC12CCC(C(=O)OC)(CC1)CC2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-4524a489f9b44534838f0c7596a9c754
CCOP(=O)(OCC)C(F)(F)c1ccc(C(=O)O)cc1Br.NCCCCc1ccccc1>>CCOP(=O)(OCC)C(F)(F)c1ccc(C(=O)NCCCCc2ccccc2)cc1Br
BrC=1C=C(C(=O)O)C=CC1C(F)(F)P(=O)(OCC)OCC.BrC=1C=C(C(=O)O)C=CC1C(F)(F)P(=O)(OCC)OCC.C(CCCC1=CC=CC=C1)N>>C(C)OP(OCC)(=O)C(F)(F)C1=C(C=C(C=C1)C(NCCCCC1=CC=CC=C1)=O)Br
O[C:16]([c:15]1[cH:14][cH:13][c:12]([C:9]([P:4]([O:3][CH2:2][CH3:1])(=[O:5])[O:6][CH2:7][CH3:8])([F:10])[F:11])[c:30]([Br:31])[cH:29]1)=[O:17].[NH2:18][CH2:19][CH2:20][CH2:21][CH2:22][c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[CH3:1][CH2:2][O:3][P:4](=[O:5])([O:6][CH2:7][CH3:8])[C:9]([F:10])([F:11])[c:12]1[cH:13][cH:...
CCOP(=O)(OCC)C(F)(F)c1ccc(C(=O)O)cc1Br.NCCCCc1ccccc1
CCOP(=O)(OCC)C(F)(F)c1ccc(C(=O)NCCCCc2ccccc2)cc1Br
null
null
null
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(NCCCCc1ccccc1)c1ccccc1
O-[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]
null
[]
null
null
null
null
The 3-bromo-4-[(diethoxyphosphoryl)difluoromethyl)benzoic acid (Compound 35) was coupled to phenbutyl amine following the procedures of Example 39 to give {[2-bromo-4-(4-phenylbutylcarbamoyl)phenyl]difluoromethyl}-phosphonic acid diethyl ester which was treated in a manner similar to Example 40 to give Compound 62. MS ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccccc1
HO-
null
null
null
CCOP(=O)(OCC)C(F)(F)c1ccc(C(=O)O)cc1Br.NCCCCc1ccccc1>>CCOP(=O)(OCC)C(F)(F)c1ccc(C(=O)NCCCCc2ccccc2)cc1Br
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2403a85443ef411082748b0d1bf65b55
CCOP([O-])OCC.O=Cc1ccc2ccccc2c1Br>>CCOP(=O)(OCC)C(O)c1ccc2ccccc2c1Br
C(C)OP(OCC)[O-].BrC1=C(C=CC2=CC=CC=C12)C=O.C(C)N(CC)CC>>C(C)OP(OCC)(=O)C(O)C1=C(C2=CC=CC=C2C=C1)Br
[CH3:1][CH2:2][O:3][P:4]([O-:5])[O:6][CH2:7][CH3:8].[CH:9](=[O:10])[c:11]1[cH:12][cH:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]2[c:20]1[Br:21]>>[CH3:1][CH2:2][O:3][P:4](=[O:5])([O:6][CH2:7][CH3:8])[CH:9]([OH:10])[c:11]1[cH:12][cH:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]2[c:20]1[Br:21]
CCOP([O-])OCC.O=Cc1ccc2ccccc2c1Br
CCOP(=O)(OCC)C(O)c1ccc2ccccc2c1Br
null
null
O1CCCC1
Miscellaneous
OtherReaction
1ffaf80f172e20da969364a5d2977299bc51b204f2262675c45c8ec58ff36ac0
e005d650d08e61fc67b766830eb53235a9bc084cc3667d2f8a73c2fb8bb34277
c1ccc2ccccc2c1
[C:1]-[#8:2]-[P;H0;D3;+0:3](-[O-;H0;D1:4])-[#8:5]-[C:6].[O;H0;D1;+0:7]=[CH;D2;+0:8]-[c:9](:[c:10]):[c:11]>>[C:1]-[#8:2]-[P;H0;D4;+0:3](=[O;H0;D1;+0:4])(-[#8:5]-[C:6])-[CH;D3;+0:8](-[OH;D1;+0:7])-[c:9](:[c:10]):[c:11]
250.6
[{"value": 250.6, "product": "C(C)OP(OCC)(=O)C(O)C1=C(C2=CC=CC=C2C=C1)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
To a solution of 1-bromo-2-naphthaldehyde (0.740 g, 0.001 mole) in tetrahydofuran (10 mL) was added triethylamine (0.150 mL, 0.001 mole) followed by diethylphosphite (0.330 mL, 0.002 mole). The reaction mixture was then stirred at room temperature under nitrogen gas for 18 hours. The volatiles then evaporated in vacuo ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Secondary alcohol
null
null
c1ccc2ccccc2c1
null
O1CCCC1
null
18
CCOP([O-])OCC.O=Cc1ccc2ccccc2c1Br>O1CCCC1>CCOP(=O)(OCC)C(O)c1ccc2ccccc2c1Br
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c53421942780463f9b28d93d665c9e04
Cc1ccc(Br)c(C(=O)O)c1.O=C(Cl)C(=O)Cl>>Cc1ccc(Br)c(C(=O)Cl)c1
BrC1=C(C(=O)O)C=C(C=C1)C.C(C(=O)Cl)(=O)Cl>>BrC1=C(C(=O)Cl)C=C(C=C1)C
O[C:8]([c:7]1[c:5]([Br:6])[cH:4][cH:3][c:2]([CH3:1])[cH:11]1)=[O:9].O=C(Cl)C(=O)[Cl:10]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([Br:6])[c:7]([C:8](=[O:9])[Cl:10])[cH:11]1
Cc1ccc(Br)c(C(=O)O)c1.O=C(Cl)C(=O)Cl
Cc1ccc(Br)c(C(=O)Cl)c1
null
CN(C=O)C
ClCCl
Functional Group Interconversion
Alcohol to chloride_Other
013cec2edeb273a7a148f349d36a52d99ff4e7bcf8eed78085df830088e387ac
aedb1f68dc5b7eb0583043e1125b741382b17974140a2f46554f0110e2ddc884
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
[]
null
null
2
HOUR
To a suspension of 2-bromo-5-methyl benzoic acid (1.0 g, 0.00465 mole) in dry dichloromethane (10 mL ) was added oxalylchloride (1.22 mL, 0.013 mole) dropwise at 0° C. followed by 1-2 drops of N,N-dimethyl formamide. The reaction mixture was then stirred for 2 hours at room temperature and the solvents were evaporated ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Carboxylic acid
Acyl halide
null
null
c1ccccc1
HCl
CN(C=O)C.ClCCl
null
2
Cc1ccc(Br)c(C(=O)O)c1.O=C(Cl)C(=O)Cl>CN(C=O)C.ClCCl>Cc1ccc(Br)c(C(=O)Cl)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b5e975d5ff7f4aa3ae29321d95a6db35
CCI.O=Cc1cc(O)ccc1Br>>CCOc1ccc(Br)c(C=O)c1
C(=O)([O-])[O-].[Cs+].[Cs+].ICC.C(=O)([O-])[O-].[Cs+].[Cs+].BrC1=C(C=O)C=C(C=C1)O>>BrC1=C(C=O)C=C(C=C1)OCC
I[CH2:2][CH3:1].[OH:3][c:4]1[cH:5][cH:6][c:7]([Br:8])[c:9]([CH:10]=[O:11])[cH:12]1>>[CH3:1][CH2:2][O:3][c:4]1[cH:5][cH:6][c:7]([Br:8])[c:9]([CH:10]=[O:11])[cH:12]1
CCI.O=Cc1cc(O)ccc1Br
CCOc1ccc(Br)c(C=O)c1
null
null
O.CS(=O)C.CCOC(=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccccc1
I-[CH2;D2;+0:1]-[C;D1;H3:2].[OH;D1;+0:3]-[c:4](:[c:5]):[c:6]>>[C;D1;H3:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:3]-[c:4](:[c:5]):[c:6]
98.2
[{"value": 98.2, "product": "BrC1=C(C=O)C=C(C=C1)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
2-Bromo-5-hydroxybenzaldehyde (0.96 g, 4.8 mmol) was dissolved in anhydrous DMSO (10 mL). Iodoethane (0.50 mL, 6.2 mmol) and Cs2CO3 (1.9 g, 6.3 mmol) were added and the mixture stirred at room temperature for 1.5 hours. Additional Cs2CO3 (1.45 g, 4.8 mmol) was added to the reaction mixture and then was stirred for 30 m...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1
HI
O.CS(=O)C.CCOC(=O)C
null
1.5
CCI.O=Cc1cc(O)ccc1Br>O.CS(=O)C.CCOC(=O)C>CCOc1ccc(Br)c(C=O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d79908969d25494b9bc412519485110e
CCOP(OCC)OCC.O=C(O)c1cc(I)ccc1Br>>CCOP(=O)(OCC)C(=O)c1cc(I)ccc1Br
BrC1=C(C(=O)O)C=C(C=C1)I.BrC1=C(C(=O)Cl)C=C(C=C1)I.BrC1=C(C(=O)Cl)C=C(C=C1)I.P(OCC)(OCC)OCC>>BrC1=C(C=C(C=C1)I)C(=O)P(OCC)(OCC)=O
CC[O:5][P:4]([O:3][CH2:2][CH3:1])[O:6][CH2:7][CH3:8].O[C:9](=[O:10])[c:11]1[cH:12][c:13]([I:14])[cH:15][cH:16][c:17]1[Br:18]>>[CH3:1][CH2:2][O:3][P:4](=[O:5])([O:6][CH2:7][CH3:8])[C:9](=[O:10])[c:11]1[cH:12][c:13]([I:14])[cH:15][cH:16][c:17]1[Br:18]
CCOP(OCC)OCC.O=C(O)c1cc(I)ccc1Br
CCOP(=O)(OCC)C(=O)c1cc(I)ccc1Br
null
null
null
Miscellaneous
OtherReaction
3c53722c63fd30e780f359165c19bae99608549d2498be52386c63534c90fc74
2464b583d940c451c00c1488740fdde63610bb85f8f9a614db893662c6ccb8a2
c1ccccc1
C-C-[O;H0;D2;+0:1]-[P;H0;D3;+0:2](-[#8:3]-[C:4])-[#8:5]-[C:6].O-[C;H0;D3;+0:7](=[O;D1;H0:8])-[c:9](:[c:10]):[c:11]>>[C:4]-[#8:3]-[P;H0;D4;+0:2](=[O;H0;D1;+0:1])(-[#8:5]-[C:6])-[C;H0;D3;+0:7](=[O;D1;H0:8])-[c:9](:[c:10]):[c:11]
null
[]
null
null
null
null
2-Bromo-5-iodobenzoic acid was converted to 2-bromo-5-iodobenzoyl chloride following procedures similar to those in Example 82A. The 2-bromo-5-iodobenzoyl chloride was reacted with triethyl phosphite following procedures similar to those in Example 82 to give diethyl (2-bromo-5-iodophenyl)oxomethylphosphonate. The diet...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
null
null
null
c1ccccc1
HO-
null
null
null
CCOP(OCC)OCC.O=C(O)c1cc(I)ccc1Br>>CCOP(=O)(OCC)C(=O)c1cc(I)ccc1Br
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d941f1079a7d416380c18f33a1dec18c
CCOP(=O)(OCC)C(F)(F)Br.Cc1ccc(I)c([N+](=O)[O-])c1>>CCOP(=O)(OCC)C(F)(F)c1ccc(C)cc1[N+](=O)[O-]
IC1=C(C=C(C=C1)C)[N+](=O)[O-].BrC(F)(F)P(OCC)(OCC)=O>>CC1=CC(=C(C=C1)C(F)(F)P(OCC)(OCC)=O)[N+](=O)[O-]
Br[C:9]([P:4]([O:3][CH2:2][CH3:1])(=[O:5])[O:6][CH2:7][CH3:8])([F:10])[F:11].I[c:12]1[cH:13][cH:14][c:15]([CH3:16])[cH:17][c:18]1[N+:19](=[O:20])[O-:21]>>[CH3:1][CH2:2][O:3][P:4](=[O:5])([O:6][CH2:7][CH3:8])[C:9]([F:10])([F:11])[c:12]1[cH:13][cH:14][c:15]([CH3:16])[cH:17][c:18]1[N+:19](=[O:20])[O-:21]
CCOP(=O)(OCC)C(F)(F)Br.Cc1ccc(I)c([N+](=O)[O-])c1
CCOP(=O)(OCC)C(F)(F)c1ccc(C)cc1[N+](=O)[O-]
null
null
null
C-C Coupling
OtherReaction
a9360a3749745f33ebc314f70b8e3a6a8dc1dd58b5ad0c0de648021793b38e59
7f4a56339ba18973720dd4919f75a8d70f3626ae8993e1433a8be25e2d9363c5
c1ccccc1
Br-[C;H0;D4;+0:1](-[F;D1;H0:2])(-[F;D1;H0:3])-[#15:4](-[#8:5])(-[#8:6])=[O;D1;H0:7].I-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11](-[#7;+:12]):[c:13]>>[#7;+:12]-[c:11](:[c:13]):[c;H0;D3;+0:8](-[C;H0;D4;+0:1](-[F;D1;H0:2])(-[F;D1;H0:3])-[#15:4](-[#8:5])(-[#8:6])=[O;D1;H0:7]):[c:9]:[c:10]
null
[]
null
null
null
null
Commercially available 4-iodo-3-nitrotoluene was reacted with diethyl bromodifluoromethylphosphonate under Cd coupling conditions using Example 25 to yield diethyl (4-methyl-2-nitrophenyl)difluoromethylphosphonate. The diethyl (4-methyl-2-nitrophenyl)difluoromethylphosphonate (500 mg, 1.55 mmol) was dissolved in EtOAc ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tertiary halide.Tertiary halide.Tertiary halide
Tertiary halide.Tertiary halide
c1ccccc1
c1ccccc1
c1ccccc1
Br-.I-
null
null
null
CCOP(=O)(OCC)C(F)(F)Br.Cc1ccc(I)c([N+](=O)[O-])c1>>CCOP(=O)(OCC)C(F)(F)c1ccc(C)cc1[N+](=O)[O-]
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-bacd7e94c6644747b69497e12a174d52
Cc1ccc([N+](=O)[O-])c(Br)c1C>>Cc1ccc(N)c(Br)c1C
C(=O)(O)[O-].[Na+].O.BrC1=C(C=CC(=C1C)C)[N+](=O)[O-].O.O.Cl[Sn]Cl>>BrC1=C(N)C=CC(=C1C)C
O=[N+:6]([O-])[c:5]1[cH:4][cH:3][c:2]([CH3:1])[c:9]([CH3:10])[c:7]1[Br:8]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([NH2:6])[c:7]([Br:8])[c:9]1[CH3:10]
Cc1ccc([N+](=O)[O-])c(Br)c1C
Cc1ccc(N)c(Br)c1C
null
null
CN(C)C=O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccccc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
To a solution of 2-bromo-3,4-dimethylnitrobenzene (1.0 g, 4.35 mmole) in 10 mL DMF was added SnCl2.2H2O (4.92 g, 21.8 mmole). This solution was stirred overnight at room temperature 50 mL of H2O was added and the pH was adjusted to 8 with the addition of sat. NaHCO3 and extracted with 150 mL of EtOAC. The organic layer...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1
Other
CN(C)C=O
null
null
Cc1ccc([N+](=O)[O-])c(Br)c1C>CN(C)C=O>Cc1ccc(N)c(Br)c1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-900acc20278b45259bc9294c07deb951
CCOC(=O)c1cnc(SC)nc1Cl.[NH4+]>>CCOC(=O)c1cnc(SC)nc1N
[NH4+].[OH-].ClC1=NC(=NC=C1C(=O)OCC)SC>>NC1=NC(=NC=C1C(=O)OCC)SC
Cl[c:13]1[c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[cH:7][n:8][c:9]([S:10][CH3:11])[n:12]1.[NH4+:14]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][n:8][c:9]([S:10][CH3:11])[n:12][c:13]1[NH2:14]
CCOC(=O)c1cnc(SC)nc1Cl.[NH4+]
CCOC(=O)c1cnc(SC)nc1N
null
null
CCO
Functional Group Interconversion
OtherReaction
1b077d7db1392b159d0fd0777de714d1fad7ef0bbe69adc404d2d103f4416610
560c85d40afb1a57d77cf3258abf3be5bba829f35224f8687bf9a1d4c1f94bd9
c1cncnc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[#16:4]):[#7;a:5]:[c:6]:[c:7]:1-[C:8](=[O;D1;H0:9])-[#8:10]-[C:11].[NH4+;D0:12]>>[#16:4]-[c:3]1:[#7;a:2]:[c;H0;D3;+0:1](-[NH2;D1;+0:12]):[c:7](-[C:8](=[O;D1;H0:9])-[#8:10]-[C:11]):[c:6]:[#7;a:5]:1
null
[]
20
CELSIUS
20
HOUR
140 ml of a 20% NH4OH solution are added, in 20 minutes, and while maintaining the temperature at around 20° C., to a suspension of 50.7 g of ethyl 4-chloro-2-(methylthio)pyrimidin-5-carboxylate in 400 ml of EtOH. After stirring at ambient temperature for 20 hours, the reaction medium is concentrated under vacuum almos...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1cncnc1
c1cncnc1
c1cncnc1
HCl
CCO
20
20
CCOC(=O)c1cnc(SC)nc1Cl.[NH4+]>CCO>CCOC(=O)c1cnc(SC)nc1N
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-721a486c34364a8f81627403375be008
NCC1CC1.O=C(O)CCNC(=O)OCC1c2ccccc2-c2ccccc21>>NCCC(=O)NCC1CC1
Cl.C1(CC1)CN.C(C)N(CC)CC.N(CCC(=O)O)C(=O)OCC1C2=CC=CC=C2C2=CC=CC=C12.C(C(=O)Cl)(=O)Cl>>C1(CC1)CNC(CCN)=O
[NH2:6][CH2:7][CH:8]1[CH2:9][CH2:10]1.O=C(OCC1c2ccccc2-c2ccccc21)[NH:1][CH2:2][CH2:3][C:4](O)=[O:5]>>[NH2:1][CH2:2][CH2:3][C:4](=[O:5])[NH:6][CH2:7][CH:8]1[CH2:9][CH2:10]1
NCC1CC1.O=C(O)CCNC(=O)OCC1c2ccccc2-c2ccccc21
NCCC(=O)NCC1CC1
null
CN(C=O)C
ClCCl
Acylation
OtherReaction
0bc677927bc73bcc6d2500d048a7a3157f92a18691a47f58331e9c6c64cbafa4
337ca72c0bb1979769aac1fc7825c6586b8e75bbb5702fd9212c320d1f1752db
C1CC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]-[NH;D2;+0:5]-C(=O)-O-C-C1-c2:c:c:c:c:c:2-c2:c:c:c:c:c:2-1.[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]-[NH2;D1;+0:5]
57.4
[{"value": 57.0, "product": "C1(CC1)CNC(CCN)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 57.4, "product": "C1(CC1)CNC(CCN)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To solution of Fmoc-β-Ala-OH (1.0 g, 3.212 mmol) and oxalyl chloride (0.428 g, 0.29 mL, 3.373 mmol) in dichloromethane (20.0 mL) was added a few drops of N,N-dimethylformamide at 0° C. The mixture was stirred at room temperature for 1 hr followed by addition of cyclopropylmethylamine (0.229 g, 0.28 mL, 3.212 mmol) and ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Carboxylic acid.Ether.Primary amine
Secondary amide.Primary amine
c1ccc2c(c1)Cc1ccccc12
null
C1CC1
HO-
CN(C=O)C.ClCCl
null
1
NCC1CC1.O=C(O)CCNC(=O)OCC1c2ccccc2-c2ccccc21>CN(C=O)C.ClCCl>NCCC(=O)NCC1CC1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-36a7c0faa6814c2c9f73edb4f607b7fd
Nc1cc(Cl)c(C(F)(F)F)cc1[N+](=O)[O-]>>Cc1cc(N)c([N+](=O)[O-])cc1C(F)(F)F
[OH-].[K+].Cl.ClC=1C(=CC(=C(C1)N)[N+](=O)[O-])C(F)(F)F.C(C)(C)(C)[O-].[K+].C(CC(=O)OCC)(=O)OCC>>CC=1C(=CC(=C(C1)N)[N+](=O)[O-])C(F)(F)F
Cl[c:2]1[cH:3][c:4]([NH2:5])[c:6]([N+:7](=[O:8])[O-:9])[cH:10][c:11]1[C:12]([F:13])([F:14])[F:15]>>[CH3:1][c:2]1[cH:3][c:4]([NH2:5])[c:6]([N+:7](=[O:8])[O-:9])[cH:10][c:11]1[C:12]([F:13])([F:14])[F:15]
Nc1cc(Cl)c(C(F)(F)F)cc1[N+](=O)[O-]
Cc1cc(N)c([N+](=O)[O-])cc1C(F)(F)F
null
null
O.CS(=O)C
Functional Group Interconversion
OtherReaction
b66818d3926a4463fb8e1c3d4a89e94e47b4d46960d4bdb7bcfbeeec427cfd4e
56de34d4a44cb25d9380269ee5e138b0f24b40a3a0db22c5508049dc775a861f
c1ccccc1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5](-[F;D1;H0:6])(-[F;D1;H0:7])-[F;D1;H0:8]):[c:9]>>[C;D1;H3:10]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5](-[F;D1;H0:6])(-[F;D1;H0:7])-[F;D1;H0:8]):[c:9]
91
[{"value": 91.0, "product": "CC=1C(=CC(=C(C1)N)[N+](=O)[O-])C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.8, "product": "CC=1C(=CC(=C(C1)N)[N+](=O)[O-])C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
20
HOUR
Under argon atmosphere, a suspension of potassium tert-butanolate (71.6 g, 625 mmol) in DMSO (150 mL) was placed in a 1.5 L flask, fitted with a mechanical stirrer. Then diethyl malonate (97.9 mL, 625 mmol) was added drop wise at 20-30° C. under ice bath cooling. To the thick white suspension was the added solid commer...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccccc1
c1ccccc1
c1ccccc1
null
O.CS(=O)C
60
20
Nc1cc(Cl)c(C(F)(F)F)cc1[N+](=O)[O-]>O.CS(=O)C>Cc1cc(N)c([N+](=O)[O-])cc1C(F)(F)F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9add6480315e46a98a360293a6be148f
Cc1cc(Br)c([N+](=O)[O-])cc1C(F)(F)F>>Cc1cc(C#N)c([N+](=O)[O-])cc1C(F)(F)F
BrC1=C(C=C(C(=C1)C)C(F)(F)F)[N+](=O)[O-].[Cu]C#N.Cl>>CC=1C(=CC(=C(C#N)C1)[N+](=O)[O-])C(F)(F)F
Br[c:4]1[cH:3][c:2]([CH3:1])[c:12]([C:13]([F:14])([F:15])[F:16])[cH:11][c:7]1[N+:8](=[O:9])[O-:10]>>[CH3:1][c:2]1[cH:3][c:4]([C:5]#[N:6])[c:7]([N+:8](=[O:9])[O-:10])[cH:11][c:12]1[C:13]([F:14])([F:15])[F:16]
Cc1cc(Br)c([N+](=O)[O-])cc1C(F)(F)F
Cc1cc(C#N)c([N+](=O)[O-])cc1C(F)(F)F
null
null
CN1C(CCC1)=O
Miscellaneous
OtherReaction
3ae4da8b7f110de99cf8afc091b6f0c8540050148e425770f8030bce1480042c
73a96fe5e833259ca394a42f82d6cc2ee7231bcde92d95030d2893b90c3fef76
c1ccccc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[C:7]#[N;D1;H0:8]):[c:2]:[c:3]
88.1
[{"value": 88.0, "product": "CC=1C(=CC(=C(C#N)C1)[N+](=O)[O-])C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 88.1, "product": "CC=1C(=CC(=C(C#N)C1)[N+](=O)[O-])C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
150
CELSIUS
30
MINUTE
A mixture of 1-bromo-5-methyl-2-nitro-4-trifluoromethyl-benzene from step 2 (49.80 g, 175 mmol) and copper(I) cyanide (16.5 g, 184 mmol) in 1-methyl-2-pyrrolidone (NMP) (180 mL) was heated up to 150° C. and stirred for 30 min under nitrogen atmosphere. The mixture was cooled to 23° C. and poured into 1 N HCl, extracted...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Nitrile
c1ccccc1
c1ccccc1
c1ccccc1
Br-
CN1C(CCC1)=O
150
0.5
Cc1cc(Br)c([N+](=O)[O-])cc1C(F)(F)F>CN1C(CCC1)=O>Cc1cc(C#N)c([N+](=O)[O-])cc1C(F)(F)F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-730d320a85e34d6b847c29289fba94a2
Cc1cc(C#N)c([N+](=O)[O-])cc1C(F)(F)F>>Cc1cc(C#N)c(N)cc1C(F)(F)F
CC=1C(=CC(=C(C#N)C1)[N+](=O)[O-])C(F)(F)F.C(C)O>>NC1=C(C#N)C=C(C(=C1)C(F)(F)F)C
O=[N+:8]([O-])[c:7]1[c:4]([C:5]#[N:6])[cH:3][c:2]([CH3:1])[c:10]([C:11]([F:12])([F:13])[F:14])[cH:9]1>>[CH3:1][c:2]1[cH:3][c:4]([C:5]#[N:6])[c:7]([NH2:8])[cH:9][c:10]1[C:11]([F:12])([F:13])[F:14]
Cc1cc(C#N)c([N+](=O)[O-])cc1C(F)(F)F
Cc1cc(C#N)c(N)cc1C(F)(F)F
null
[Fe]
Cl.CO
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccccc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
78.4
[{"value": 78.0, "product": "NC1=C(C#N)C=C(C(=C1)C(F)(F)F)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.4, "product": "NC1=C(C#N)C=C(C(=C1)C(F)(F)F)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
1
HOUR
Iron powder (37.42 g, 670 mmol) was added in small portions to a stirred suspension of finely grinded 5-methyl-2-nitro-4-trifluoromethyl-benzonitrile from step 3 (34.58 g, 150 mmol) in methanol (75 mL) and 37% HCl (93 mL). The internal temperature was kept between 40 and 60° C. by external water bath cooling. The resul...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1
Other
[Fe].Cl.CO
50
1
Cc1cc(C#N)c([N+](=O)[O-])cc1C(F)(F)F>[Fe].Cl.CO>Cc1cc(C#N)c(N)cc1C(F)(F)F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2dad9ca12f0a4cdebbe56d3a67afacc9
Cc1cc(C#N)c(N)cc1C(F)(F)F>>Cc1cc(C#N)ccc1C(F)(F)F
N(=O)OCCC(C)C.NC1=C(C#N)C=C(C(=C1)C(F)(F)F)C.N(=O)OCCC(C)C>>CC=1C=C(C#N)C=CC1C(F)(F)F
N[c:7]1[c:4]([C:5]#[N:6])[cH:3][c:2]([CH3:1])[c:9]([C:10]([F:11])([F:12])[F:13])[cH:8]1>>[CH3:1][c:2]1[cH:3][c:4]([C:5]#[N:6])[cH:7][cH:8][c:9]1[C:10]([F:11])([F:12])[F:13]
Cc1cc(C#N)c(N)cc1C(F)(F)F
Cc1cc(C#N)ccc1C(F)(F)F
null
null
CC(C)(C)OC.C1CCOC1
Reduction
OtherReaction
a069304de6b46c6d557b2e80c544464adc3bb98001f26c098e87c25f29d552f9
a4f16f822d2806606c05d0c4baa1761ad37a11006840dde863a01a253bdff5dd
c1ccccc1
N-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[cH;D2;+0:1]:[c:2]:[c:3]
92.8
[{"value": 92.8, "product": "CC=1C=C(C#N)C=CC1C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
23
CELSIUS
null
null
To a solution of 2-amino-5-methyl-4-trifluoromethyl-benzonitrile from step 4 (23.34 g, 117 mmol) in dry THF (350 mL) was added isoamyl nitrite (34.3 mL, 257 mmol) and the mixture was refluxed for 20 h. Additional isoamyl nitrite (16.6 mL, 129 mmol) was added and the mixture was refluxed for further 20 h. The mixture wa...
10.6084/m9.figshare.5104873.v1
null
Primary amine
null
c1ccccc1
c1ccccc1
c1ccccc1
Other
CC(C)(C)OC.C1CCOC1
23
null
Cc1cc(C#N)c(N)cc1C(F)(F)F>CC(C)(C)OC.C1CCOC1>Cc1cc(C#N)ccc1C(F)(F)F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d44c2f7f507240709e8ec1b0f10585dd
Cc1cc(C#N)ccc1C(F)(F)F.[OH-]>>Cc1cc(C(=O)O)ccc1C(F)(F)F
CC=1C=C(C#N)C=CC1C(F)(F)F.[OH-].[Na+].O1CCOCC1.Cl>>CC=1C=C(C(=O)O)C=CC1C(F)(F)F
N#[C:5][c:4]1[cH:3][c:2]([CH3:1])[c:10]([C:11]([F:12])([F:13])[F:14])[cH:9][cH:8]1.[OH-:7]>>[CH3:1][c:2]1[cH:3][c:4]([C:5](=[O:6])[OH:7])[cH:8][cH:9][c:10]1[C:11]([F:12])([F:13])[F:14]
Cc1cc(C#N)ccc1C(F)(F)F.[OH-]
Cc1cc(C(=O)O)ccc1C(F)(F)F
null
null
CC(C)(C)OC
Acylation
OtherReaction
e05c34ebe51fe654c61f91bb118ee544dcd0a035df9f073c07f2e1b77a1f299a
e722778fc7d66899e0f2f256942c8c213a77617f32bb1410d97747833c62e260
c1ccccc1
N#[C;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].[OH-;D0:5]>>[O;D1;H0:6]=[C;H0;D3;+0:1](-[OH;D1;+0:5])-[c:2](:[c:3]):[c:4]
null
[]
23
CELSIUS
null
null
A mixture of 3-methyl-4-trifluoromethyl-benzonitrile from step 5 (16.25 g, 88 mmol) and 3 N NaOH (88 mL, 264 mmol) in dioxane (90 mL) was refluxed for 18 h. The mixture was cooled to 23° C., diluted with TBME, acidified with 1 N HCl to pH 1 and extracted twice with TBME. The combined organic layers were washed with bri...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Carboxylic acid
null
null
c1ccccc1
null
CC(C)(C)OC
23
null
Cc1cc(C#N)ccc1C(F)(F)F.[OH-]>CC(C)(C)OC>Cc1cc(C(=O)O)ccc1C(F)(F)F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-0fae13e3e41e4091b3c9f1fcfac1c4e2
CNOC.Cc1cc(C(=O)O)ccc1C(F)(F)F>>CON(C)C(=O)c1ccc(C(F)(F)F)c(C)c1
CC=1C=C(C(=O)O)C=CC1C(F)(F)F.Cl.CNOC.CN1CCOCC1.Cl.CN(CCCN=C=NCC)C>>CON(C(C1=CC(=C(C=C1)C(F)(F)F)C)=O)C
[CH3:1][O:2][NH:3][CH3:4].O[C:5](=[O:6])[c:7]1[cH:8][cH:9][c:10]([C:11]([F:12])([F:13])[F:14])[c:15]([CH3:16])[cH:17]1>>[CH3:1][O:2][N:3]([CH3:4])[C:5](=[O:6])[c:7]1[cH:8][cH:9][c:10]([C:11]([F:12])([F:13])[F:14])[c:15]([CH3:16])[cH:17]1
CNOC.Cc1cc(C(=O)O)ccc1C(F)(F)F
CON(C)C(=O)c1ccc(C(F)(F)F)c(C)c1
null
CN(C)C=1C=CN=CC1
CC(C)(C)OC.CN(C)C=O.C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Carboxylic Acids
ac72df6259d5d7baee7abdbd4706ef4b4627f86ead9dc94f0cefcfcb37c21def
c5e4172490b2731ba9322b68af56376edadc31ce0bb9a3dfdea23a1817a852fd
c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C;D1;H3:6]-[#8:7]-[NH;D2;+0:8]-[C;D1;H3:9]>>[C;D1;H3:6]-[#8:7]-[N;H0;D3;+0:8](-[C;D1;H3:9])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
null
[]
23
CELSIUS
18
HOUR
To a suspension of 3-methyl-4-trifluoromethyl-benzoic acid from step 6 (14.1 g, 69.1 mmol), N,O-dimethylhydroxylamine hydrochloride (10.78 g, 111 mmol), N-methylmorpholine (12.14 mL, 111 mmol) and 4-DMAP (844 mg, 691 mmol) in DCM (230 mL) at 0° C. were added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Tertiary amide
null
null
c1ccccc1
HO-
CN(C)C=1C=CN=CC1.CC(C)(C)OC.CN(C)C=O.C(Cl)Cl
23
18
CNOC.Cc1cc(C(=O)O)ccc1C(F)(F)F>CN(C)C=1C=CN=CC1.CC(C)(C)OC.CN(C)C=O.C(Cl)Cl>CON(C)C(=O)c1ccc(C(F)(F)F)c(C)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-07273519cc5a420d9b55a2a52a879b30
CON(C)C(=O)c1ccc(C(F)(F)F)c(C)c1>>CC(=O)c1ccc(C(F)(F)F)c(C)c1
Cl.CON(C(C1=CC(=C(C=C1)C(F)(F)F)C)=O)C.C[Mg]Br.C(C)OCC>>CC=1C=C(C=CC1C(F)(F)F)C(C)=O
CON(C)[C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]([C:8]([F:9])([F:10])[F:11])[c:12]([CH3:13])[cH:14]1>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]([C:8]([F:9])([F:10])[F:11])[c:12]([CH3:13])[cH:14]1
CON(C)C(=O)c1ccc(C(F)(F)F)c(C)c1
CC(=O)c1ccc(C(F)(F)F)c(C)c1
null
null
CCOC(=O)C.C1CCOC1
Functional Group Interconversion
OtherReaction
0e1b501f4aadb0e84ffc93b33216cc37dfe617cb6c3e325779c58539a7f5c4e4
af85307a4412ed48cedcfde84079732215472ffbe274bdc1dc12e9979d5c5e06
c1ccccc1
C-O-N(-C)-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]>>[C;D1;H3:6]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
null
[]
0
CELSIUS
1
HOUR
To a solution of N-methoxy-3,N-dimethyl-4-trifluoromethyl-benzamide from step 7 (16.90 g, 68.36 mmol) in THF (280 mL) at −5° C. was added a 3 M methylmagnesium bromide solution in diethyl ether (45.6 mL, 136.7 mmol). The mixture was stirred at 0° C. for 1 h, then was warmed up to 23° C. and stirring was continued at 23...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Ketone
null
null
c1ccccc1
HO-
CCOC(=O)C.C1CCOC1
0
1
CON(C)C(=O)c1ccc(C(F)(F)F)c(C)c1>CCOC(=O)C.C1CCOC1>CC(=O)c1ccc(C(F)(F)F)c(C)c1