反应详情

To phosphorus trichloride (775.4 g, 5.5 M, 10% molar excess) was added dropwise with stirring over two hours a solution of neopentylene glycol (520.8 g, 5.0 M) in chloroform (1200 ml). After the slight endotherm and evolution of HCl had subsided, the clear colorless solution was freed of most of the chloroform and excess PCl3 by distillation at atmospheric pressure to a pot temperature of 100° C. Distillation of the residue through a short vacuum-jacketed Vigreaux column yielded 803.6 g (95.3% yield) of 2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane (III), bp 65° C./10 mm nD25 1.4738, % Cl found 20.71 (21.03 calculated).

1. distillationby distillation at atmospheric pressure to a pot temperature of 100° C
2. distillationDistillation of the residue through a short vacuum-jacketed Vigreaux column