Ammonia → HCID 178507981, compound

Participants

Reaction Steps

4.3 g (0.25 mol) of gaseous ammonia were passed into a mixture of 23.3 g (0.1 mol) of 2,4-dichloro-6-trifluoromethoxypyrimidine in 150 ml of methyl tert-butyl ether in the course of 45 minutes at from -50° to -45° C. while stirring. Stirring was continued for 30 minutes at -50° C., one hour at -30° C. and one hour at 25° C. The precipitate which had separated out was filtered off under suction, washed with water and dried, 5.4 g (33.1% of theory) of 4-amino-2,4-dichloropyrimidine of melting point 270°-272° C. being obtained as a byproduct. The filtrate was washed with water, dried, partially evaporated down under reduced pressure and chromatographed using 5:1 petroleum ether/ether, 3 g (12.8% of theory) of starting material being obtained as a colorless oil in the first fractions and 9 g (42% of theory) of the title compound being obtained as colorless crystals of melting point 55°-56° C. in the subsequent fraction. The conversion was 48.3%.

Provenance & Evidence