HRID273848

反应详情

EQUATION

反应方程式

HRID 273848 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-methoxy-2-(2,2,2-trifluoroethoxy)benzene (3.83 g) in dry methylene chloride (50 ml) was added boron tribromide (3.1 ml) with stirring under ice cooling, and the mixture was reacted for 30 minutes. The reaction mixture was poured into an aqueous sodium bicarbonate solution (500 ml), and the mixture was extracted with diethyl ether. The extract was washed with water, dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by medium pressure liquid column chromatography on silica gel using a mixture of hexane and diethyl ether (20/1) as eluent to give 2.37 g of 2-(2,2,2-trifluoroethoxy)phenol melting at 49°-50° C.

WORKUP

后处理

  1. customthe mixture was reacted for 30 minutes
  2. extractionthe mixture was extracted with diethyl ether
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by medium pressure liquid column chromatography on silica gel using
  7. additiona mixture of hexane and diethyl ether (20/1) as eluent