反应详情

6 g of t-butyl peroctoate in 30 g of methane phosphonous acid methyl ester and 116 g of 1-methyl-1-oxophospholine are added dropwise to 282 g of oxygen-free methane phosphonous acid methyl ester at 120° C with stirring. The reaction time is 90 minutes. Excess methane phosphonous acid methyl ester and a small quantity of 1-methyl-oxophospholine are distilled off. The residue, consisting of 205 g of 1-methyl-1-oxophospholanylmethyl phosphinic acid methyl ester, is purified by distillation under vacuum (bp 1mm :210° to 220° C) to yield 186 g of pure product which solidifies very slowly to stellate crystals which begin to reliquefy at 70° C. Acid saponification leads to isomeric 1-methyl-1-oxophospholanyl-methyl phosphinic acids of the idealized constitution: ##STR16##

1. distillationExcess methane phosphonous acid methyl ester and a small quantity of 1-methyl-oxophospholine are distilled off
2. distillationis purified by distillation under vacuum (bp 1mm :210° to 220° C)