Reacción #63668

ord-d57e115760924d43a21fc3df3125c5f3

Condiciones de reacción

Temperatura
65°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroIn a four necked 100 ml flask equipped with a condenser, a dropping funnel
  2. 2
    Otrowas continued at the same temperature as above for 3 hours
  3. 3
    workup.STIRRINGwhile stirring
  4. 4
    Lavadowas washed with an alkaline solution
  5. 5
    Otrodried with alumina
  6. 6
    Temperaturacooled
  7. 7
    workup.DISTILLATIONThe resultant liquid was distilled

Procedimiento

In a four necked 100 ml flask equipped with a condenser, a dropping funnel and a thermometer, tributylamine (20.0 g, 108 mmoles) was charged and warmed to 65° C. Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate (4.88 g, 20 mmol) was dropwise added thereto while stirring. The reaction was continued at the same temperature as above for 3 hours while stirring. The gas evolved from a top of the condenser was washed with an alkaline solution, dried with alumina and cooled. The resultant liquid was distilled to give 2-trifluoromethyl-3,3,3-trifluoropropene (2.49 g). Yield, 76 %.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04766238uspto-grants-1988_08