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In a nitrogen atmosphere 100 g of methane-phosphonous acid mono-n-butyl ester are heated to 140° C. while stirring. Over a period of 2 hours a mixture of 85 g of methallyl carbamate and 3.7 g of tert.butyl perbenzoate is added dropwise and stirring is continued for 1 hour at 135° C. Distillation is then started up to an internal temperature of 140° C. and at 0.8 torr, whereby about 5 g of distillate are obtained. 180 g of (3-carbamoyloxy-2-methyl-propyl)methyl-phosphinic acid n-butyl ester are obtained, ND23 : 1.4725, corresponding to a yield of about 95% of the theory. ##STR7##

1. additionis added dropwise
2. stirringstirring
3. distillationDistillation
4. customis then started up to an internal temperature of 140° C. and at 0.8 torr, whereby about 5 g of distillate
5. customare obtained