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
- 30 °C
PROCEDURE
实验过程
To a suspension of lithium aluminum hydride (0.424 g) in tetrahydrofuran (20 mL), a solution of the compound obtained from step c above (2 g) in tetrahydrofuran (10 mL) was added at −20° C. The reaction mixture was stirred for 2 hours at 30° C. and a saturated solution of sodium sulphate was added at the same temperature. The reaction mixture was then filtered through a celite pad and the residue was washed with ethyl acetate. The organic layer was dried over anhydrous sodium sulphate, filtered, and concentrated under reduced pressure. The residue thus obtained was purified by column chromatography over silica gel using 50% ethyl acetate in hexane as eluant to afford the title compound (1.2 g).
WORKUP
后处理
- filtrationThe reaction mixture was then filtered through a celite pad
- washthe residue was washed with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue thus obtained
- customwas purified by column chromatography over silica gel using 50% ethyl acetate in hexane as eluant