HRID1438896
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling
- distillationits contents distilled
- customUnconverted trichloromethane phosphonic dichloride sublimed between 70° and 125°
- distillationThe continued distillation