反应详情

温度

140 °C

0.47 g (0.0013 mol) of 4-tert-butyl-N-(6-chloro-2-methyl-amino-pyrimidin-4-yl)-benzenesulfonamide was dissolved in 10 ml of ethanol, treated with 1.3 g (0.019 mol) of methylamine hydrochloride and 4.7 ml (0.034 mol) of triethylamine and stirred in an autoclave at 140° C. for 18 hours. The mixture was freed completely from solvent, the residue was partitioned in ethyl acetate/water and the insoluble constituents were filtered off under suction. The filtered cake was recrystallized in methanol/diethyl ether. There was obtained 0.15 g (33%) of N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-tert-butyl-benzenesulfonamide as white crystals; m.p. 316-318° C.

1. customthe residue was partitioned in ethyl acetate/water
2. filtrationthe insoluble constituents were filtered off under suction
3. customThe filtered cake was recrystallized in methanol/diethyl ether