反应详情

温度

250 °C

In a 100 mL Monel autoclave were mixed 1.99 g (11.0 mmol) of 4-morpholinylmethylphosphonic acid and 13.1 g (165 mmol) of a 50.3% solution of NaOH to give a slurry. The reaction vessel was sealed and heated to 250° C. for two hours. There was only a small increase in internal pressure during the heating period. The temperature of the reaction was then raised to 300° C. for three hours. In the span of this heating period the internal pressure rose from 2.4×106N/M2 to 4.0×106N/M2. The reaction was cooled to room temperature and the residual internal pressure was vented off. The reaction mixture, which consisted of a white slurry, was diluted with 10 mL of water and neutralized by the addition of 13.6 mL of conc. HCl. The resulting solution was concentrated to dryness. The residue was taken up in conc. HCl and the precipitated NaCl was filtered away. The final filtrate was concentrated and purified by ion exchange chromatography (Dowex 50X8-400) to yield 0.82 g (44.1%) of N-phosphonomethylglycine (NMR, D2O) δ 4.07 (s, 2H), 3.25 (d, J=12 Hz, 2H) and 0.40 g (32.8%) of aminomethylphosphonic acid (NMR, D2O) δ 3.06 (d, J=12 Hz, 2H) based on the amount of starting substrate.

1. customto give a slurry
2. customThe reaction vessel was sealed
3. temperaturea small increase in internal pressure during the heating period
4. temperatureThe temperature of the reaction was then raised to 300° C. for three hours
5. temperatureThe reaction was cooled to room temperature
6. concentrationThe resulting solution was concentrated to dryness
7. filtrationthe precipitated NaCl was filtered away
8. concentrationThe final filtrate was concentrated
9. custompurified by ion exchange chromatography (Dowex 50X8-400)