반응 #530962

반응 방정식

phosphorous acid

trioxane

acetonitrile

phosphorus trichloride

→

N-acetylaminomethane phosphonic acid

반응 조건

후처리

1. 1
   온도The resulting mixture is heated
2. 2
   온도under reflux for about two hours
3. 3
   기타A 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
   기타precipitates
8. 8
   여과a white crystalline product which is filtered off
9. 9
   건조dried at 60° C. in a water jet vacuum

실험 절차

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.

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