Réaction #530962

Équation de réaction

phosphorous acid

trioxane

acetonitrile

phosphorus trichloride

→

N-acetylaminomethane phosphonic acid

Conditions de réaction

Traitement

1. 1
   TempératureThe resulting mixture is heated
2. 2
   Températureunder reflux for about two hours
3. 3
   AutreA highly viscous oil separates as a result of the reaction
4. 4
   workup.DISTILLATIONUnreacted acetonitrile is distilled off
5. 5
   workup.DISSOLUTIONThe residue is dissolved in a small amount of water
6. 6
   workup.ADDITIONAddition of acetone
7. 7
   Autreprecipitates
8. 8
   Filtrationa white crystalline product which is filtered off
9. 9
   Séchagedried at 60° C. in a water jet vacuum

Mode opératoire

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.

Source