反应详情

82 g of aqueous phosphorous acid and 32 g of trioxane are dissolved in 200 cc of acetonitrile. 5 cc of phosphorus trichloride are added to said solution. The resulting mixture is heated to boiling under reflux for about two hours. A highly viscous oil separates as a result of the reaction. Unreacted acetonitrile is distilled off. The residue is dissolved in a small amount of water. Addition of acetone precipitates therefrom a white crystalline product which is filtered off and dried at 60° C. in a water jet vacuum. About 100 g of N-acetylaminomethane phosphonic acid are obtained. By thin layer chromatographic investigation of the filtrate it was found that, in addition to phosphorous acid, the solution still contained some additional N-acetylaminomethane phosphonic acid and also another phosphonic acid which apparently is N-acetylimino-bis-methane phosphonic acid.

1. temperatureThe resulting mixture is heated
2. temperatureunder reflux for about two hours
3. customA highly viscous oil separates as a result of the reaction
4. distillationUnreacted acetonitrile is distilled off
5. dissolutionThe residue is dissolved in a small amount of water
6. additionAddition of acetone
7. customprecipitates
8. filtrationa white crystalline product which is filtered off
9. dry with materialdried at 60° C. in a water jet vacuum