反应详情

A mixture of diethyl 3-[N-(p-methoxybenzyloxy)-N-tosylamino]propylphosphonate (3.0 g), 6 N hydrochloric acid (25 ml) and acetic acid (25 ml) was refluxed with stirring for 12 hours. The resultant mixture was concentrated under reduced pressure to give a brownish oily residue. The residue was washed with ethyl ether (100 ml), and then water (100 ml) was added thereto with stirring. Insoluble materials were filtered off from the mixture, whereafter the filtrate was washed with ethyl ether, and then treated with an activated charcoal. The aqueous solution was concentrated under reduced pressure to give a faint yellowish oily residue. The residue was allowed to stand overnight in desiccator under reduced pressure to give crystals. The crystals were washed with ethyl ether to give p-toluene sulfonic acid salt of 3-(N-hydroxyamino)propylphosphonic acid (1.50 g) in the form of fiant yellowish crystals. MP: 129°-135° C.

1. temperaturewas refluxed
2. concentrationThe resultant mixture was concentrated under reduced pressure
3. customto give a brownish oily residue
4. washThe residue was washed with ethyl ether (100 ml)
5. additionwater (100 ml) was added
6. stirringwith stirring
7. filtrationInsoluble materials were filtered off from the mixture, whereafter the filtrate
8. washwas washed with ethyl ether
9. additiontreated with an activated charcoal
10. concentrationThe aqueous solution was concentrated under reduced pressure
11. customto give a faint yellowish oily residue
12. waitto stand overnight in desiccator under reduced pressure
13. customto give crystals
14. washThe crystals were washed with ethyl ether