Vinyl Fluoride → Tris(pentafluoroethyl)phosphane

HRID 1272578노트

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HRID 1272578 반응식
F[P:2](F)([C:17]([F:23])([F:22])[C:18]([F:21])([F:20])[F:19])([C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])[C:3]([F:9])([F:8])[C:4]([F:7])([F:6])[F:5].C([SiH](CC)CC)C.FC=C>>[F:9][C:3]([P:2]([C:10]([F:15])([F:16])[C:11]([F:12])([F:13])[F:14])[C:17]([F:23])([F:22])[C:18]([F:21])([F:20])[F:19])([F:8])[C:4]([F:7])([F:6])[F:5]

참가 물질

4

반응물 3

HCID 6339Vinyl FluorideHCID 12052TriethylsilaneHCID 10287940Difluorotris(pentafluoroethyl)phosphorane

생성물 1

HCID 15809510Tris(pentafluoroethyl)phosphane수율 82.8%

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온도
-20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9caa25636ccf47819d92dab8e758b67f
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07208626B2

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