Reacción #4836

ord-30de9da655d044c9895a8b402380e49a

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04727187uspto-grants-1988_02