4,5-Dichloro-4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolane → 4,5-Difluoro-2,2-bis(trifluoromethyl)-1,3-dioxole

Participants

Reaction Conditions

Reaction Steps

A solution of bromine (3 g) and tetrahydrofuran (30 mL) was slowly added to a well stirred mixture of magnesium turnings (25 g) and tetrahydrofuran (365 mL) at 20° C. After the exothermic reaction stopped, the reaction mixture was cooled to 28° C. and 133 g of the 4,5-dichloro-perfluoro-2,2-dimethyl-1,3-dioxolane (89.9% trans and 10.1% cis) was slowly added. After an induction period an exothermic reaction was observed. The reaction mixture was distilled to remove all material boiling up to 65° C. The distillate was washed with ice water to give 58.9 g perfluoro-2,2-dimethyl-1,3-dioxole.

Provenance & Evidence