反应详情

To a mixture of hemiaminal A1 (2.0 g, 4.2 mmol) in dichloromethane (20 mL) was added thionyl chloride (1.5 mL, 12.6 mmol) and stirred for 2 h at room temperature. To the reaction mixture was added methanol (10 mL) and stirred a further 2 h. The reaction poured into NaHCO3 (aq) and extracted with dichloromethane. The organic phase dried over MgSO4, evaporated and the residue purified on silica eluting with 1:1:0.1 dichloromethane/ethyl acetate/methanol to give the title compound as a cream solid (1.3 g, 63%).

1. stirringstirred a further 2 h
2. extractionextracted with dichloromethane
3. dry with materialThe organic phase dried over MgSO4
4. customevaporated
5. customthe residue purified on silica eluting with 1:1:0.1 dichloromethane/ethyl acetate/methanol