HRID1706197
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed
- concentrationThe resultant mixture was concentrated under reduced pressure
- additionto the residue was added water
- concentrationThe mixture was concentrated under reduced pressure
- customto give a residue, which
- washwas washed with acetonitrile
- dissolutiondissolved in water (10 ml)
- additionTo the solution were added pyridine (800 ml) and ethanol (4 ml)
- waitto stand overnight at 4° C.