反应详情

温度

250 °C

To a 100 mL Monel autoclave were added 2.23 g (12.3 mmol) of 4-morpholinylmethylphosphonic acid 7.88 g (98.5 mmol) of a 50% solution of NaOH, and 10 mL of H2O to give a slurry. The vessel was flushed with N2, sealed and heated to 250° C. This temperature was maintained for five and one-half hours with little noticeable reaction occurring. The temperature was then raised to 300° C. for three hours. During this period the internal pressure in the vessel rose from 4.5×106N/M2 to 5.7×106N/M2. The vessel was cooled to room temperature and the residual pressure was released. The resulting solution was diluted with water and neutralized with 8.1 mL (98.5 mmol) of conc. HCl. The 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 to yield 0.71 g (34.1 %) of N-phosphonomethylglycine and 0.43 g (31.5%) of aminomethylphosphonic acid.

1. customto give a slurry
2. customThe vessel was flushed with N2
3. customsealed
4. temperatureThis temperature was maintained for five and one-half hours with little noticeable reaction
5. temperatureThe temperature was then raised to 300° C. for three hours
6. waitDuring this period the internal pressure in the vessel rose from 4.5×106N
7. temperatureThe vessel was cooled to room temperature
8. concentrationThe solution was concentrated to dryness
9. filtrationthe precipitated NaCl was filtered away
10. concentrationThe final filtrate was concentrated
11. custompurified by ion exchange chromatography