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 continued for 1 hour in each case at -70° C., 0° C. and 25° C. The reaction mixture was evaporated down under reduced pressure, after which the residue was stirred with water, the solution was extracted twice with ethyl acetate and the extract was dried over magnesium sulfate. It was partially evaporated down under reduced pressure and then subjected to fractional chromatography 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