反应详情

To a stirred solution of oxetan-3-one (1 g, 13.87 mmol) in methanol (40 mL) was added 2-(tert-butyl-dimethylsilanyloxy)-ethylamine (2.7 mg, 15.27 mmol). The mixture was stirred for 30 min at room temperature after cooling, Na(CN)BH3 was added portion-wise, followed by stirring at room temperature for 2 h. The reaction mixture was quenched with water, extracted with dichloromethane (3×30 mL). The organic part was concentrated, dried and purified by Combi-Flash column (eluted at 20-50% ethyl acetate in hexane) to get [2-(tert-butyl-dimethylsilanyloxy)-ethyl]-oxetan-3-yl-amine (8 g) (1.5 g, 46.71%) as a light yellow oil.

1. temperatureafter cooling
2. stirringby stirring at room temperature for 2 h
3. customThe reaction mixture was quenched with water
4. extractionextracted with dichloromethane (3×30 mL)
5. concentrationThe organic part was concentrated
6. customdried
7. custompurified by Combi-Flash column (eluted at 20-50% ethyl acetate in hexane)