反应详情

温度

5 °C

11 g (0.1 mol) of diphosphorus trioxide (P2O3) were dissolved in 70 ml of tetrahydrofuran and the solution was cooled to 5° C. 30.2 g (0.2 mol) of N-hydroxymethylbenzamide were then added in portions at 5°-10° C. in the course of 30 minutes with stirring and under a nitrogen atmosphere. The mixture was then allowed to come to room temperature with stirring and was then heated to reflux for 2 hours; a clear solution was not formed in this case. After cooling to room temperature, 4.5 g (0.25 mol) of water were added dropwise at 30°-40° C. and the mixture was then heated to reflux for 1 hour. It was then cooled, additionally stirred and filtered with suction. 28.5 g of benzoylaminomethanephosphonic acid having a melting point of 171° to 173° C. were obtained. A further 5 g were isolated from the mother liquor. Altogether, 33.5 g (78% of theory) of product were thus obtained.

1. customto come to room temperature
2. stirringwith stirring
3. temperaturewas then heated
4. temperatureto reflux for 2 hours
5. customa clear solution was not formed in this case
6. temperatureAfter cooling to room temperature
7. temperaturethe mixture was then heated
8. temperatureto reflux for 1 hour
9. temperatureIt was then cooled
10. stirringadditionally stirred
11. filtrationfiltered with suction