反应 #4836

反应方程式

4-(1,1-dichloro-2,2,2-trifluoroethoxy)chlorobenzene

hydrogen fluoride

antimony pentachloride

→

4-(1-chloro-1,2,2,2-tetrafluoroethoxy)chlorobenzene

收率 89.8%

反应条件

后处理

1. 1
   其他A 500 ml polytetrafluoroethylene reactor equipped with stirrer
2. 2
   温度thermometer and reflux condenser
3. 3
   其他The resultant hydrogen chloride is removed from the reactor through the reflux condenser
4. 4
   其他Excess hydrogen fluoride is removed by distillation
5. 5
   workup.DISSOLUTIONthe residue is dissolved in 200 ml of methylene chloride
6. 6
   萃取the solution is extracted with water
7. 7
   其他The organic phase is separated by distillation

实验过程

A 500 ml polytetrafluoroethylene reactor equipped with stirrer, thermometer and reflux condenser is charged with 55.9 g (0.2 mol) of 4-(1,1-dichloro-2,2,2-trifluoroethoxy)chlorobenzene in 100 ml of hydrogen fluoride. 3.0 g (0.01 mol; corresponding to 5 mol%) of antimony pentachloride are added at a temperature in the range from -5° C. to 0° C. The resultant hydrogen chloride is removed from the reactor through the reflux condenser. After 20 minutes at 0° C., the evolution of hydrogen chloride ceases. Excess hydrogen fluoride is removed by distillation, the residue is dissolved in 200 ml of methylene chloride and the solution is extracted with water. The organic phase is separated by distillation, affording 47.3 g (89.8% of theory) of 4-(1-chloro-1,2,2,2-tetrafluoroethoxy)chlorobenzene. Boiling point 181° C., nD25 =1.4362.

来源