反应详情

14.5 g (53.7 mmol) of 3-ethoxycarbonyl-phenyl-guanidine nitrate, 11.3 g (53.7 mmol) of 3-dimethylamino-1-(2-chloro4-pyridyl)-2-propen-1-one and 2.4 g (60 mmol) of sodium hydroxide are stirred in 150 ml of isobutanol for 14 hours at 110°. After cooling, washing twice with 100 ml of ethanol each time and crystallising (tetra-hydrofuran/ethanol), N-[3-ethoxycarbonyl-phenyl]-4-(2-chloro4-pyridyl)-2-pyrimidineamine is obtained; m.p. 149°-150°, FAB-MS: 355 (M+ +H).

1. temperatureAfter cooling
2. washwashing twice with 100 ml of ethanol each time
3. customcrystallising (tetra-hydrofuran/ethanol)