Ammonia → HCID 86614658, compound

HRID 1983852Notes

Reaction equation

HRID 1983852 reaction equation
CC(C)=O.[Cl:5][C:6]1[CH:15]=[C:14]2[C:9]([C:10]([C:32]3[CH:33]=[C:34](/[CH:38]=[CH:39]/[C:40]([OH:42])=[O:41])[CH:35]=[CH:36][CH:37]=3)=[C:11]([CH2:17][C:18]([NH:20][C:21]3[CH:26]=[CH:25][C:24]([F:27])=[CH:23][C:22]=3[C:28]([F:31])([F:30])[F:29])=[O:19])[C:12](=[O:16])[O:13]2)=[CH:8][C:7]=1[CH3:43].C(O)C.[NH3:47]>O>[Cl:5][C:6]1[CH:15]=[C:14]2[C:9]([C:10]([C:32]3[CH:33]=[C:34](/[CH:38]=[CH:39]/[C:40]([O-:42])=[O:41])[CH:35]=[CH:36][CH:37]=3)=[C:11]([CH2:17][C:18]([NH:20][C:21]3[CH:26]=[CH:25][C:24]([F:27])=[CH:23][C:22]=3[C:28]([F:29])([F:31])[F:30])=[O:19])[C:12](=[O:16])[O:13]2)=[CH:8][C:7]=1[CH3:43].[NH4+:47]

Participants

5

Reactant 3

HCID 222AmmoniaHCID 702EthanolHCID 86614657HCID 86614657, compound

Product 1

HCID 86614658HCID 86614658, compoundYield 90.1%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

A mixture of (2E)-3-{3-[7-chloro-3-(2-{[4-fluoro-2-(trifluoromethyl)phenyl]amino}-2-oxoethyl)-6-methyl-2-oxo-2H-chromen-4-yl]phenyl}acrylic acid acetone solvate (6.18 g), ethanol (56 ml) and water (11 ml) was heated to 60° C., and 5% aqueous ammonia (6 ml) was added dropwise thereto with stirring to dissolve the mixture. The solution was concentrated under reduced pressure and crystals obtained were dried at 45° C. for 8 hours under reduced pressure to obtain the title compound as colorless crystals (5.20 g, yield 90.1%).

Workup

  1. dissolutionto dissolve the mixture
  2. concentrationThe solution was concentrated under reduced pressure and crystals
  3. customobtained
  4. customwere dried at 45° C. for 8 hours under reduced pressure

Sources & evidence

ORD record
ord-bd1bf3bc1b884bf49e29852d2e357ba4
Source dataset
uspto-grants-2009_06
Patent number
US07541478B2

Reaction notes

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