反应详情

500 g (3.75 mol) of AlCl3 (Aldrich-99% pure) was stirred mechanically under N2 in a r.b. flask fitted with a -80° C. condenser while 1750 mL (~2625 g, 19 mol) of CFCl3 was added over a 1.5-hr period. Reaction is very exothermic in the early stages, so addition of CFCl3 was slow at first in order to keep the temperature below 65° C., then rapid. The resulting suspension was stirred an additional 3 hrs while volatiles (CF2Cl2) were allowed to escape through the warmed condenser. The condenser was then replaced with a simple stillhead, and most of the CCl4 was distilled under reduced pressure [mainly bp 38° C. (200 mm)]. Finally, the last traces of volatiles were removed by warming the residual solid to 30°-35° C. at 0.05 mm.

1. additionwas added over a 1.5-hr period
2. customReaction
3. customthe temperature below 65° C.
4. distillationmost of the CCl4 was distilled under reduced pressure [mainly bp 38° C. (200 mm)]
5. customFinally, the last traces of volatiles were removed
6. temperatureby warming the residual solid to 30°-35° C. at 0.05 mm