反应 #4837

反应方程式

1,1-dichloro-2,2,2-trifluoroethylthiobenzene

hydrogen fluoride

antimony pentachloride

→

1-chloro-1,2,2,2-tetrafluoroethylthiobenzene

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
   workup.ADDITIONafter 4 hours a further 2.8 g (10 mol%) of antimony pentachloride are added
5. 5
   其他After a total reaction time of 5 hours, the hydrogen fluoride is removed by distillation
6. 6
   workup.DISSOLUTIONthe residue is dissolved in 150 ml of methylene chloride
7. 7
   萃取the solution is extracted with water
8. 8
   其他The solution is separated by distillation

实验过程

A 500 ml polytetrafluoroethylene reactor equipped with stirrer, thermometer and reflux condenser is charged with 24.7 g (0.094 mol) of 1,1-dichloro-2,2,2-trifluoroethylthiobenzene which are subsequently condensed with 50 g of hydrogen fluoride. 4.2 g (0.014 mol; corresponding to 15 mol%) of antimony pentachloride are added at a temperature of 20° C. The resultant hydrogen chloride is removed from the reactor through the reflux condenser. After 3 hours a further 1.4 g (5 mol%) and after 4 hours a further 2.8 g (10 mol%) of antimony pentachloride are added. After a total reaction time of 5 hours, the hydrogen fluoride is removed by distillation, the residue is dissolved in 150 ml of methylene chloride and the solution is extracted with water. The solution is separated by distillation, affording 1-chloro-1,2,2,2-tetrafluoroethylthiobenzene. Boiling point 178°-179° C., nD20 =1.4732.

来源