Water → HCID 178518629, compound

Participants

Reaction Conditions

Reaction Steps

Alternatively, the title compound can be preferably prepared as follows: A mixture of ethyl 4-(4-chloro-2-aminobenzoyl)-3-trifluoromethyl-1H-pyrazole-5-carboxylate (1.0 g, 2.76 mmol), ammonium acetate (0.21 g, 2.76 mmol) and 1-methyl-2-pyrrolidinone (2.3 mL) was heated with stirring at 160° C. under N2 for one hour. After cooling to room temperature, water (25 mL) was added to the stirred reaction mixture. The resulting aqueous mixture was filtered after stirring for ten minutes. The filter cake was washed with water (2×25 mL) then dried under vacuum to give a tan solid. The solid was placed in methylene chloride (25 mL) and the mixture was stirred for fifteen minutes, then filtered. The filter cake was washed with methylene chloride (2×25 mL) and dried under vacuum to give the title compound as a tan solid (0.66 g, 76%, m.p. 334-336° C.).

Provenance & Evidence