Trichlorofluoromethane → AlCl3 CFCl3
Reaction equation
[Al+3:1].[Cl-:2].[Cl-].[Cl-].[C:5]([Cl:9])([Cl:8])([Cl:7])[F:6].C(Cl)([Cl:13])(F)F>>[Al+3:1].[Cl-:7].[Cl-:13].[Cl-:2].[C:5]([Cl:9])([Cl:8])([Cl:7])[F:6]Participants
4
Conditions
- Temperature
- 32.5 °C
Procedure
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.