HRID580363

反应详情

EQUATION

反应方程式

HRID 580363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

38.5 g (0.34 mol) phenylphosphine dissolved in 40 ml toluene was added at 25° C. to a suspension of 160 g PCl5 (0.77 mol) in 500 ml toluene. After the exothermal reaction had subsided, the whole was heated to 70° C. until gas ceased to be evolved. The low boilers were removed under vacuum. The crude product yield was 67 g; 31P-NMR: δ P=161 ppm, C6H5PCl2, 94.4 mol%. The residue was distilled under vacuum. bp 98° C./17 mbar; yield: 50.6 g (81% of the theoretical).

WORKUP

后处理

  1. customAfter the exothermal reaction
  2. customThe low boilers were removed under vacuum
  3. distillationThe residue was distilled under vacuum