HRID1706197

反应详情

EQUATION

反应方程式

HRID 1706197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of dibutyl 3-[N-isobutoxycarbonyl-N-(p-methoxybenzyloxy)amino]propylphosphonate (6.04 g), conc. hydrochloric acid (60 ml) and acetic acid (60 ml) was refluxed with stirring for 21 hours. The resultant mixture was concentrated under reduced pressure, and to the residue was added water. The mixture was concentrated under reduced pressure to give a residue, which was washed with acetonitrile and then dissolved in water (10 ml). To the solution were added pyridine (800 ml) and ethanol (4 ml), and then the mixture was allowed to stand overnight at 4° C. to give 3-(N-hydroxyamino)propylphosphonic acid (1.02 g) in the form of crystals. MP: 160°-166° C. (dec.).

WORKUP

后处理

  1. temperaturewas refluxed
  2. concentrationThe resultant mixture was concentrated under reduced pressure
  3. additionto the residue was added water
  4. concentrationThe mixture was concentrated under reduced pressure
  5. customto give a residue, which
  6. washwas washed with acetonitrile
  7. dissolutiondissolved in water (10 ml)
  8. additionTo the solution were added pyridine (800 ml) and ethanol (4 ml)
  9. waitto stand overnight at 4° C.