HRID30601

反应详情

EQUATION

反应方程式

HRID 30601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturewarmed to room temperature
  2. stirringstirred vigorously for 1 h at room temperature
  3. customThe phases are separated
  4. extractionThe aqueous phase is extracted with CH2Cl2
  5. washwashed with NaHCO3 and brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo
  8. customThe resultant residue is purified by column chromatography (5% EtOAc and hexane