تفاعل #4836

معادلة التفاعل

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

hydrogen fluoride

antimony pentachloride

→

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

المردود 89.8%

ظروف التفاعل

المعالجة

1. 1
   أخرىA 500 ml polytetrafluoroethylene reactor equipped with stirrer
2. 2
   درجة الحرارةthermometer and reflux condenser
3. 3
   أخرىThe resultant hydrogen chloride is removed from the reactor through the reflux condenser
4. 4
   أخرىExcess hydrogen fluoride is removed by distillation
5. 5
   workup.DISSOLUTIONthe residue is dissolved in 200 ml of methylene chloride
6. 6
   استخلاصthe solution is extracted with water
7. 7
   أخرىThe organic phase is separated by distillation

الإجراء التجريبي

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.

المصدر