Methylamine → HCID 21996923, compound

Participants

Reaction Conditions

Reaction Steps

At -70° to -60° C. and over a period of 30 minutes, 5.8 g (0.188 mol) of gaseous methylamine was added, with stirring, to 20.3 g (0.0938 mol) of 4-chlorodifluoromethoxy-2,6-difluoropyrimidine in 150 ml of tetrahydrofuran. The mixture was stirred for 1 hour at -70° C., 1 hour at 0° C. and 1 hour at 25° C., and then evaporated down under reduced pressure. The residue was stirred with water and extracted twice with ethyl acetate, and the extract was dried over magnesium sulfate. It was evaporated down, partially under reduced pressure, and then fractionally chromatographed over silica gel (1:5 ether/ligroin mixture). The first fractions contained the title compound (melting point 57°-61° C.) in a yield of 12.5 g (58.5%).

Provenance & Evidence