HRID30601
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
A solution of (R)-2-fluoro-2-(3-bromophenyl)acetaldehyde in CH2Cl2 and ethanol is treated with NaBH4 (189 mg, 5 mmol), stirred for 30 min, cooled to 0° C., treated with saturated NH4Cl, warmed to room temperature, stirred vigorously for 1 h at room temperature and diluted with CH2Cl2. The phases are separated. The aqueous phase is extracted with CH2Cl2. The organic phase and the extracts are combined, washed with NaHCO3 and brine, dried over MgSO4 and concentrated in vacuo. The resultant residue is purified by column chromatography (5% EtOAc and hexane as eluant)to give (R)-2-fluro-2-(3-bromophenyl)-1-ethanol.
WORKUP
后处理
- temperaturewarmed to room temperature
- stirringstirred vigorously for 1 h at room temperature
- customThe phases are separated
- extractionThe aqueous phase is extracted with CH2Cl2
- washwashed with NaHCO3 and brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe resultant residue is purified by column chromatography (5% EtOAc and hexane