反应详情

A total of 116 g of 1-methyl-1-oxophospholine and 6 g of tert.-butyl peroctoate in 30 g of methane phosphonous acid methyl ester are simultaneously added dropwise with stirring at 120° C to 282 g of oxygen-free methane phosphonous acid methyl ester. The reaction time is 90 minutes. Excess methane phosphonous acid methyl ester and a little 1-methyl oxophospholine are distilled off. For purification, the residue of 205 g of 1-methyl-1-oxophospholanyl methyl phosphinic acid methyl ester is distilled in vacuo (b.p. 210° -220° C) and gives 186 g of a pure product which hardens very slowly into star-shaped crystals which become liquid again at a temperature above 70° C.

1. distillationExcess methane phosphonous acid methyl ester and a little 1-methyl oxophospholine are distilled off
2. customFor purification
3. distillationthe residue of 205 g of 1-methyl-1-oxophospholanyl methyl phosphinic acid methyl ester is distilled in vacuo (b.p. 210° -220° C)