HRID485224

反应详情

EQUATION

反应方程式

HRID 485224 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

19.8 g (0.1 mol) dicyclohexylphosphane was added dropwise at room temperature to 26.1 g (0.11 mol) hexachloroethane. After the exothermal reaction which took place with evolution of HCl was terminated, the reaction mixture was stirred for 3 hours at 100° C. The yields (31 -P-NMR) were as follows: δ P=125.2 ((C6H11)2PCl, 94 wgt %); δ P=194.4 (C6H11PCl2, 2 wgt %); δ P=76.7 ((C6H11)2P(O)Cl, 4 wgt %). The crude product was distilled and 13.7 g (59 wgt %) dicyclohexylchlorophosphane (bp.: 136°-138° C./4 millibars) was obtained.

WORKUP

后处理

  1. customAfter the exothermal reaction which
  2. customwas terminated
  3. customThe yields (31 -P-NMR)
  4. distillationThe crude product was distilled