HRID1350875
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
To a tetrahydorofran (THF) (20 ml) solution of 7-methoxy-4,4-dimethylchroman-2-one (4.1 g, 19.7 mmol) was added lithium aluminum hydride (750 mg, 19.7 mmol) at 0° C. The reaction mixture was stirred at 0° C. for 1 hour. To the mixture was added H2O (1 ml) carefully to form a white prepicitate. The organic layer was dried over magnesium sulfate. After filtration to separate solvent and magnesium sulfate and precipitate, the solvent was removed under reduced pressure to give a residue, which was applied to a silica gel chromatography column and eluted with ethyl acetate/hexane=¼ to furnish 3.0 g (76% yield) of the title compound as colorless oil.
WORKUP
后处理
- customto form a white prepicitate
- dry with materialThe organic layer was dried over magnesium sulfate
- filtrationAfter filtration
- customto separate solvent and magnesium sulfate and precipitate
- customthe solvent was removed under reduced pressure
- customto give a residue, which
- washeluted with ethyl acetate/hexane=¼