Ammonia → HCID 11274841, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 4-{3-[7-chloro-3-(2-{[4-fluoro-2-(trifluoromethyl)phenyl]amino}-2-oxoethyl)-6-methyl-2-oxo-2H-chromen-4-yl]phenyl}butanoic acid obtained in Reference Example 9 (26.7 g, 0.0463 mol) in acetone (534 ml) was added 25% aqueous ammonia (4 ml) at 50° C., and the mixture was stirred at the same temperature for 15 minutes. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in a mixture of acetonitrile (534 ml) and water (107 ml). The reaction mixture was heated to 70° C., and a solution of calcium chloride (3.14 g, 0.0255 mol) in water (107 ml) was slowly added dropwise thereto. The reaction mixture was stirred at 70° C. for 3.5 hours, water (214 ml) was added thereto and the mixture was further stirred at 70° C. for 1 hour and at room temperature for 12 hours. Crystals obtained were collected by filtration, washed with water (100 ml) and dried at 50° C. under reduced pressure to obtain the title compound (26.67 g).

Provenance & Evidence