반응 #2633
ord-e7b93282e05f4addbe5f6faab80d2b9a
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반응 조건
후처리
- 1기타model autoclave fitted with a condenser
- 2기타was evacuated
- 3온도cooled to about -40° C.
- 4온도The temperature was increased to 120° C.
- 5온도maintained at that temperature for a total of 22 h
- 6기타was attached to two -78° C.
실험 절차
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%.