Ammonia → HCID 21996901, compound

Participants

Reaction Conditions

Reaction Steps

At -75° to -70° C. and over a period of 1 hour, 9.8 g (0.578 mol) of gaseous ammonia was gassed while stirring into a mixture of 62.5 g (0.289 mol) of 2,4-difluoro-6-chlorodifluoromethoxypyrimidine in 300 ml of tetrahydrofuran. The mixture was stirred for 1 hour at -70° C. and then heated to room temperature. The precipitate was suction filtered, partitioned between ethyl acetate and water, and the organic phase was dried over magnesium sulfate. The reaction filtrate was evaporated down, dissolved in the abovementioned ethyl acetate phase, chromatographed over silica gel (5:1 ligroin/ether mixture) and evaporated down. There was obtained 46.5 g (75.3% of theory) of the title compound as colorless crystals of melting point 77°-80° C.

Provenance & Evidence