反应详情

温度

-20 °C

56.0 g (131.4 mmol) of difluorotris(pentafluoroethyl)phosphorane and 38.0 g (326.8 mmol) of triethylsilane were refluxed with vigorous stirring for 12 hours in an FEP (fluoroethylene polymer) flask at a bath temperature of 110° C. The reaction mixture was subsequently distilled under atmospheric pressure under an inert-gas atmosphere, and 48.0 g of the fraction having a boiling range of 81–85° C. were collected. This fraction was subsequently cooled to −20° C., and the lower phase (desired product) was separated off. 42.2 g of virtually pure tris(pentafluoroethyl)phosphine were obtained, corresponding to a yield of 82.8%, based on the difluorotris(pentafluoroethyl)phosphorane employed.

1. distillationThe reaction mixture was subsequently distilled under atmospheric pressure under an inert-gas atmosphere, and 48.0 g of the fraction
2. customwere collected
3. customthe lower phase (desired product) was separated off