HRID1438896

反应详情

EQUATION

反应方程式

HRID 1438896 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.6 g (0.1 mole)butene-1, 71 g (0.3 mole) trichloromethane phosphonic dichloride and 0.5 g tert. butyl perbenzoate were heated in 100 ml methylene chloride in a closed ampoule and in the absence of air, during 10 hours at 120°. After cooling, the ampoule was opened and its contents distilled. Unconverted trichloromethane phosphonic dichloride sublimed between 70° and 125° at 25 mm pressure. The continued distillation yielded 10.3 g 1.1,3-trichloropentane-1-phosphonic dichloride, bp/0.05: 64° -66°. Found Cl: 61.3% Calc. for C5H8Cl5OP: 61.0%.

WORKUP

后处理

  1. temperatureAfter cooling
  2. distillationits contents distilled
  3. customUnconverted trichloromethane phosphonic dichloride sublimed between 70° and 125°
  4. distillationThe continued distillation