Dichloromethane → 1.1,3-Trichloropentane-1-phosponic dichloride

Participants

Reaction Steps

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-phosponic dichloride, bp/0.05: 64°-66°. Found Cl: 61.3%. Calc. for C5H8Cl5OP: 61.0%.

Provenance & Evidence