HRID380019
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
Solid sodium borohydride (11.8 g) was added with cooling in three portions over 3 days to a stirred solution of (2S)-2-(4-bromophenoxy)-3-methylbutanoic acid, methyl ester (27.7 g) in ethanol (400 ml). The reaction was concentrated under reduced pressure and the residue partitioned between 2M hydrochloric acid (400 ml) and ether. The organic layer was dried over anhydrous magnesium sulfate filtered and concentrated under reduced pressure. The residue was purified by column chromatography over silica gel eluting with dichloromethane:isohexane (1:1) to give the sub-title compound as an oil (13.7 g).
WORKUP
后处理
- concentrationThe reaction was concentrated under reduced pressure
- customthe residue partitioned between 2M hydrochloric acid (400 ml) and ether
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography over silica gel eluting with dichloromethane:isohexane (1:1)