HRID704778
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
PROCEDURE
实验过程
To a solution of 2,2-diethyl-3,4-dihydro-4-oxo-2H-1-benzopyran-6-carbonitrile (2.29 g) in a mixture of methanol (23 ml) and tetrahydrofuran (5 ml) was added sodium borohydride (0.37 g) at ambient temperature. The reaction mixture was stirred for an hour at the same temperature and evaporated in vacuo. The residue was dissolved in ethyl acetate, and then washed with water and brine successively. The extract was dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was purified with silica gel column chromatography using a mixture of methanol and methylene chloride (1:20) as an eluent to give 2,2-diethyl-3,4-dihydro-4-hydroxy-2H-1-benzopyran-6-carbonitrile (2.34 g).
WORKUP
后处理
- customevaporated in vacuo
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with water and brine successively
- dry with materialThe extract was dried over anhydrous magnesium sulfate
- customevaporated in vacuo
- customThe residue was purified with silica gel column chromatography
- additiona mixture of methanol and methylene chloride (1:20) as an eluent