反应详情

A solution of 2-(chloromethyl)pyrimidin-4-amine 126 (30.0 g, 209 mmol), morpholine 63 (23.7 g, 272 mmol) and triethylamine (42.3 g, 418 mmol) in anhydrous ethanol (250 mL) was heated at reflux for 16 h. The solvent was removed in vacuo and methanol (400 mL), H2O (100 mL) and sodium bicarbonate (25.0 g) were added. Stirring was continued for 30 min. The mixture was concentrated and purified by flash chromatography (dichloromethane: methanol: triethylamine=100:8:0.5) to give 127 (25.0 g, 62% yield).

1. temperatureat reflux for 16 h
2. customThe solvent was removed in vacuo and methanol (400 mL), H2O (100 mL) and sodium bicarbonate (25.0 g)
3. additionwere added
4. concentrationThe mixture was concentrated
5. custompurified by flash chromatography (dichloromethane: methanol: triethylamine=100:8:0.5)