Reaktion #4836

Reaktionsgleichung

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

hydrogen fluoride

antimony pentachloride

→

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

Ausbeute 89.8%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA 500 ml polytetrafluoroethylene reactor equipped with stirrer
2. 2
   Temperaturthermometer and reflux condenser
3. 3
   SonstigeThe resultant hydrogen chloride is removed from the reactor through the reflux condenser
4. 4
   SonstigeExcess hydrogen fluoride is removed by distillation
5. 5
   workup.DISSOLUTIONthe residue is dissolved in 200 ml of methylene chloride
6. 6
   Extraktionthe solution is extracted with water
7. 7
   SonstigeThe organic phase is separated by distillation

Vorschrift

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.

Quelle