HRID1691825
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 1-(5-amino-4-bromo-2-chloro-phenyl)-ethanone (0.25 g, 1.00 mmol) in methanol (5 ml) was added NaBH4 (0.076 g, 2.01 mmol). The mixture was stirred at room temperature for two hours, then quenched by addition of 2N HCl and taken to neutral pH with pH7 buffer. The mixture was extracted with dichloromethane, and the combined organic layers were washed with water and brine, dried over MgSO4, filtered and concentrated to dryness under reduced pressure. Purification of the residue by flash chromatography (hex:EtOAc/7:3) gave 1-(5-amino-4-bromo-2-chloro-phenyl)-ethanol 0.195 g (77%) as a clear oil.
WORKUP
后处理
- customquenched by addition of 2N HCl
- extractionThe mixture was extracted with dichloromethane
- washthe combined organic layers were washed with water and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure
- customPurification of the residue by flash chromatography (hex:EtOAc/7:3)