HRID248806

反应详情

EQUATION

反应方程式

HRID 248806 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of catechol (5.5 g) and 4-(trifluoromethyl)acetophenone (10.3 g) in toluene (150 ml) containing a catalytic amount (0.2 g) of p-toluenesulphonic acid monohydrate was heated under reflux for 3 days. Water produced in the condensation was separated by means of a Dean-Stark trap. After removal of the solvent under reduced pressure, the residue was purified by chromatography on silica gel using methylene chloride as eluant. Pure 2-methyl-2-[4-(trifluoromethyl)phenyl]-1,3-benzodioxole was obtained as a colourless oil (10.8 g, 77%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 days
  3. customwas separated by means of a Dean-Stark trap
  4. customAfter removal of the solvent under reduced pressure
  5. customthe residue was purified by chromatography on silica gel