HRID1706220

反应详情

EQUATION

反应方程式

HRID 1706220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Formic acid (300 mg.) was added dropwise to acetic anhydride (330 mg.) with stirring and the mixture was stirred for half an hour. To this solution were added 2-hydroxy-3-(N-hydroxyamino)propylphosphonic acid (430 mg.) and then formic acid (0.5 ml.), and the mixture was stirred for 1.5 hours at ambient temperature and then evaporated to dryness under reduced pressure. The oily residue was dissolved in methanol (10 ml.) and adjusted to pH 6-7 with conc. aqueous ammonium hydroxide solution to give oily precipitates which was collected by decantation and pulverized by triturating with methanol to give monoammonium salt of 3-(N-formyl-N-hydroxyamino)-2-hydroxypropylphosphonic acid (80 mg.).

WORKUP

后处理

  1. stirringthe mixture was stirred for half an hour
  2. customevaporated to dryness under reduced pressure
  3. dissolutionThe oily residue was dissolved in methanol (10 ml.)
  4. customto give oily
  5. customprecipitates which
  6. customwas collected by decantation
  7. customby triturating with methanol