Ethyl 4,4,4-trifluoroacetoacetate → HCID 178516594, compound

Participants

Reaction Conditions

Reaction Steps

Ethyl trifluoroacetoacetate (1.50 g, 8.15 mmol) was added to a solution of 3-(1-phenylpiperidin-4-yl)-1H-pyrazol-5-amine (648 mg, 2.67 mmol) produced in Reference Example 3 in acetic acid (10 mL), and the mixture was stirred at 60° C. for 2 hours and 30 minutes. A saturated sodium bicarbonate aqueous solution was added to the reaction solution, followed by extraction with ethyl acetate. The obtained organic layer was washed with brine and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography [NH-silica gel column, elute: ethyl acetate/methanol=100/0-96/4 (gradient)] and further purified by silica gel chromatography [elute: hexane/ethyl acetate=60/40-0/100 (gradient)] to obtain the title compound (430 mg, yield: 42%).

Provenance & Evidence