1,1,1,2-tetrachloro-2,2-difluoroethane

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 2.0 g (18.3 mmol) of p-aminophenol was added over a period of 10 minutes to a mixture of 0.48 g (20.1 mmol) of sodium hydride in 20 ml of dry DMSO. The mixture was stirred for 20 minutes. 3.73 g (18.3 mmol) of 1,1-difluoro-tetrachloroethane was added causing an exotherm to 47° C. The mixture was stirred at 60° C. for 2 hours, then poured into ice water. The brown solid was collected by filtration, dried, dissolved in ether and then HCl gas was bubbled into the solution causing the above-named aniline to precipitate as the hydrochloride salt. The white solid (4.4 g, 87 percent of theoretical d 250° C.) was collected by filtration. to 47° C The mixture was stirred at 60° C. for 2 hours The brown solid was collected by filtration dried dissolved in ether HCl gas was bubbled into the solution to precipitate as the hydrochloride salt The white solid (4.4 g, 87 percent of theoretical d 250° C.) was collected by filtration

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 37.5 g of 3,3-dimethyl-4-pentenoic acid methyl ester, 102 g of 1,1,1,2-tetrachloro-2,2-difluoroethane, 22 g of acetonitrile, 325 mg of FeCl3.6H2O, 255 mg of benzoin and 200 mg of dimethylamine hydrochloride were heated to 100°-120° C. in a 250 ml VA autoclave under 6 bars of nitrogen for 7 hours. Distillation of the mixture gave 3,3-dimethyl-4,6,6,7-tetrachloro-7,7-difluoroenanthic acid methyl ester of boiling point 129°-134° C./0.7-0.9 m bar. Refractive index: nD20 =1.4680. ##STR8## Distillation of the mixture