Hydrofluoric Acid → 1-Chloro-1,2,2,2-tetrafluoroethylthiobenzene

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.

1. customA 500 ml polytetrafluoroethylene reactor equipped with stirrer
2. temperaturethermometer and reflux condenser
3. customThe resultant hydrogen chloride is removed from the reactor through the reflux condenser
4. additionafter 4 hours a further 2.8 g (10 mol%) of antimony pentachloride are added
5. customAfter a total reaction time of 5 hours, the hydrogen fluoride is removed by distillation
6. dissolutionthe residue is dissolved in 150 ml of methylene chloride
7. extractionthe solution is extracted with water
8. customThe solution is separated by distillation

ORDレコード

ord-53a85923a86c4172acc0fb7d8d5d8d30

出典データセット

uspto-grants-1988_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04727187