Ethyl 4,4,4-trifluoroacetoacetate → HCID 178516598, compound

Participants

Reaction Conditions

Reaction Steps

Ethyl trifluoroacetoacetate (5.64 mL, 38.5 mmol) was added to a solution of 3-{1-[4-(difluoromethoxy)phenyl]piperidin-4-yl}-1H-pyrazol-5-amine (2.97 g, 9.63 mmol) produced in Reference Example 72 in acetic acid (52 mL), and the mixture was stirred at 60° C. for 3 hours. The reaction solution was cooled to room temperature, and the solvent was distilled off under reduced pressure, followed by azeotropy with toluene twice. The obtained residue was purified by silica gel column chromatography [NH-silica gel column, elute: hexane/ethyl acetate=100/0-0/100 (gradient)] and further purified by silica gel column chromatography [elute: hexane/ethyl acetate=100/0-40/60 (gradient)] to obtain the title compound (1.84 g, yield: 43%).

Provenance & Evidence