HRID1691825

反应详情

EQUATION

反应方程式

HRID 1691825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customquenched by addition of 2N HCl
  2. extractionThe mixture was extracted with dichloromethane
  3. washthe combined organic layers were washed with water and brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure
  7. customPurification of the residue by flash chromatography (hex:EtOAc/7:3)