二环己基膦 → 二环己基氯化膦

HRID 580364

反应方程式

HRID 580364 反应方程式
[CH:1]1([PH:7][CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.P(Cl)(Cl)(Cl)(Cl)[Cl:15]>C1(C)C=CC=CC=1>[CH:8]1([P:7]([CH:1]2[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2)[Cl:15])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1

参与物

4

反应物 2

HCID 13239二环己基膦HCID 24819五氯化磷

产物 1

HCID 2734135二环己基氯化膦

试剂、催化剂与溶剂 1

HCID 1140甲苯溶剂2 次

实验过程

A solution of 19 g (0.1 mol) dicyclohexylphosphine in 50 ml toluene was dropped into a suspension of 21 g (0.1 mol) PCl5 in 100 ml toluene. The reaction temperature was maintained at less than 30° C. After all had been dropped in, the whole was boiled for 1 hour under reflux. A slight precipitate was removed by means of a reverse frit and the reaction mixture was freed from all low boilers at 60° C. under 0.1 mbar. Yield: 23.3 g; 31P-NMR: δ P=126 ppm, (c-C6H11)2PCl, 96 mol %; δ P=54 ppm, (c-C6H11)2P(O)Cl, 3.7 mol %.

后处理

  1. temperatureThe reaction temperature was maintained at less than 30° C
  2. additionAfter all had been dropped in, the whole
  3. temperatureunder reflux
  4. customA slight precipitate was removed by means of a reverse frit
  5. customwas freed from all low boilers at 60° C. under 0.1 mbar

来源与证据

ORD记录
ord-3c747dcb9a764531aa7d598f1c5b78dd
来源数据集
uspto-grants-1988_06
专利号
US04752648

关联笔记

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