HCID 10175375, compound → HCID 87716473, compound

HRID 2252014Notes

Reaction equation

HRID 2252014 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[N:9]=[N:10][N:11]([CH2:19][C:20]3[CH:25]=[C:24]([C:26]([F:29])([F:28])[F:27])[CH:23]=[C:22]([C:30]([F:33])([F:32])[F:31])[CH:21]=3)[C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:3]=1[C:34]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=1[Cl:42])=[O:35]>C(OCC)(=O)C.CCCCCCC.O>[OH2:35].[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[N:9]=[N:10][N:11]([CH2:19][C:20]3[CH:25]=[C:24]([C:26]([F:27])([F:28])[F:29])[CH:23]=[C:22]([C:30]([F:32])([F:31])[F:33])[CH:21]=3)[C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:3]=1[C:34]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=1[Cl:42])=[O:35].[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[N:9]=[N:10][N:11]([CH2:19][C:20]3[CH:25]=[C:24]([C:26]([F:27])([F:28])[F:29])[CH:23]=[C:22]([C:30]([F:32])([F:31])[F:33])[CH:21]=3)[C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:3]=1[C:34]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=1[Cl:42])=[O:35]

Participants

5

Reactant 1

HCID 10175375HCID 10175375, compound

Product 1

HCID 87716473HCID 87716473, compound

Reagents, catalysts & solvents 3

HCID 962WaterSolventHCID 8857Ethyl AcetateSolventHCID 8900HeptaneSolvent2×

Procedure

Dissolve {4-amino-2-[1-(3,5-bistrifluoromethylbenzyl)-5-phenyl-1H-[1,2,3]triazol-4-yl]-pyridin-3-yl}-(2-chlorophenyl)-methanone (582 g, 0.97 mol) in ethyl acetate (1880 mL), heptane (1990 mL) and water (90 mL) at 70° C. Cool to room temperature and stir for 18.5 hours. Add heptane (3980 mL) dropwise over 4 hours. Filter and dry in a vacuum oven at 40° C. for approximately 15 hours to give the title compound. Kf=1.52%.

Workup

  1. filtrationFilter
  2. customdry in a vacuum oven at 40° C. for approximately 15 hours

Sources & evidence

ORD record
ord-c780c7f04788462585b7e87b21832290
Source dataset
uspto-grants-2008_01
Patent number
US07320994B2

Reaction notes

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