Reacción #2633

ord-e7b93282e05f4addbe5f6faab80d2b9a

Ecuación de reacción

Condiciones de reacción

Temperatura
-10°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otromodel autoclave fitted with a condenser
  2. 2
    Otrowas evacuated
  3. 3
    Temperaturacooled to about -40° C.
  4. 4
    TemperaturaThe temperature was increased to 120° C.
  5. 5
    Temperaturamaintained at that temperature for a total of 22 h
  6. 6
    Otrowas attached to two -78° C.

Procedimiento

A 600 mL, magnetically stirred, model autoclave fitted with a condenser (maintained at -10° C.), was evacuated, cooled to about -40° C., and charged with 0.6.9 g (0.036 mol) TiCl4 followed by 64 g (0.255 mol) CCl3CH2CCl3, and 102.5 g (5 mol) HF. The temperature was increased to 120° C. and maintained at that temperature for a total of 22 h. During the heating period, pressure in excess of 400 psig was periodically vented to an aqueous KOH scrubber which was attached to two -78° C. cold traps. At the end of the heating period, the remainder of the autoclave contents were slowly vented. The cold traps contained 36.1 g material which by GC analysis, contained 14.5% CF3CH2CF3 and 84.0% CF3CH2 CF2Cl, corresponding to a yield for CF3CH2CF2Cl of 69%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05728904uspto-grants-1998_03