反应详情

43.2 g (0.424 mol) of acetic anhydride were cooled to 10° C. A solution of 28.2 g (0.2 mol) of benzenephosphonous acid in 40 ml acetic acid were then added dropwise at 15° C., with stirring and cooling. After this, 30.2 g (0.2 mol) of N-hydroxymethylbenzamide were added in portions in the course of 10 minutes at 15° C., with cooling. After this, the cooling was removed, during which process the internal temperature rose to 35° C. After this, the mixture was refluxed for 3 hours and subsequently cooled. 175 ml of water were then added; during this process, the temperature rose to 35° C. The mixture was refluxed again, and finally cooled again, with stirring. After crystallisation, a total of 40 g (73% of theory) of benzoylaminomethylphenylphosphinic acid of a melting point of 158°-160° C. were obtained. CHNP analysis revealed:

1. temperaturecooling
2. temperaturewith cooling
3. customAfter this, the cooling was removed, during which process the internal temperature
4. customrose to 35° C
5. temperatureAfter this, the mixture was refluxed for 3 hours
6. temperaturesubsequently cooled
7. addition175 ml of water were then added
8. customrose to 35° C
9. temperatureThe mixture was refluxed again
10. temperaturefinally cooled again
11. stirringwith stirring
12. customAfter crystallisation