HRID374845

反应详情

EQUATION

反应方程式

HRID 374845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

51 g of 2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 2 or 17 were dissolved in 300 ml of carbon tetrachloride, and 0.5 g of anhydrous FeCl3 was added. 32 g of bromine were then added and the mixture was stirred under reflux for 3 hours. After cooling, the mixture was washed with 10% strength NaHSO3 solution, dried with MgSO4 and distilled. The yield was 49 g (63% of theory), and the boiling point was 94°-98° C. under 8 mbar.

WORKUP

后处理

  1. temperatureunder reflux for 3 hours
  2. temperatureAfter cooling
  3. washthe mixture was washed with 10% strength NaHSO3 solution
  4. dry with materialdried with MgSO4
  5. distillationdistilled