Ammonia → HCID 21996901, compound

Participants

Reaction Steps

9.8 g (0.578 mol) of gaseous ammonia were passed into a mixture of 62.5 g (0.289 mol) of 2,4-difluoro-6-chlorodifluoromethoxypyrimidine in 300 ml of tetrahydrofuran at from -75° to -70° C. in the course of one hour while stirring. Stirring was continued for one hour at -70° C., after which the mixture was warmed up to room temperature. The precipitate which had separated out was filtered off under suction and partitioned between ethyl acetate and water and the organic phase was dried over mangesium sulfate. The reaction filtrate was evaporated down, the residue was dissolved in the above ethyl acetate phase, the solution was chromatographed over silica gel using 5:1 petroleum ether/ether and the eluate was evaporated down. 46.5 g (75.3% of theory) of the title compound were obtained as colorless crystals of melting point 77°-80° C.

Provenance & Evidence