反应 #1633095
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07632969B2
反应条件: temp:-20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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. The reaction mixture was subsequently distilled under atmospheric pressure under an inert-gas atmosphere, and 48.0 g of the fraction were collected the lower phase (desired product) was separated off
来源 ID: ord-d7e8c2d38dff4016b88fc7be3b70ef6a