Methylamine → HCID 21996923, compound

Participants

Reaction Steps

20.3 g (0.0938 mol) of 4-chlorodifluoromethoxy-2,6-difluoropyrimidine in 150 ml of tetrahydrofuran were initially taken and 5.8 g (0.188 mol) of gaseous methylamine were added at from -70° to -60° C. in the course of 30 minutes while stirring. Stirring was carried out for 1 hour at -70° C., for 1 hour at 0° C. and for 1 hour at 25° C. After the reaction mixture had been 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 partially evaporated down under reduced pressure and then chromatographed over silica gel using 1:5 ether/petroleum ether. The first fractions contained the title compound of melting point 57°-61° C. in a yield of 12.5 g (58.5%).

Provenance & Evidence