HRID1369619
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A solution of Example 61A (254 mg, 0.793 mmol) in absolute ethanol (4 mL) was treated with anhydrous CaCl2 (177 mg, 1.59 mmol), stirred for 1 hour, cooled to 0° C., treated with NaBH4 (123 mg, 3.25 mmol), stirred at 0° C. for 4 hours and at room temperature for 18 hours, treated with water and extracted with dichloromethane. The extract was washed with brine, dried (Na2SO4), filtered and concentrated. The residue was purified on silica gel with 30% ethyl acetate/hexane to provided the title compound.
WORKUP
后处理
- stirringstirred at 0° C. for 4 hours and at room temperature for 18 hours
- extractionextracted with dichloromethane
- washThe extract was washed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified on silica gel with 30% ethyl acetate/hexane