HRID325528

反应详情

EQUATION

反应方程式

HRID 325528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 14.5 g. (0.13 mole) of isooxazolidine hydrochloride in water (100 ml.) is added 10.4 g. (0.13 mole) of fifty percent (w/w) aqueous sodium hydroxide and the mixture stirred for fifteen minutes. To this solution is added 18.1 g. (0.065 moles) of 2-methyl-2-thiopseudourea sulfate and the entire mixture stirred under a stream of nitrogen overnight. The mixture is refluxed for 11/2 hours, then filtered while still hot. The water is removed under vacuum to give a semi-solid residue which is triturated with hot isopropanol (3×100 ml.). The isopropanol is removed under vacuum to give an oil which is crystallized from isopropanol to give N-amidinoisooxazolidine sulfate.

WORKUP

后处理

  1. additionTo this solution is added 18.1 g
  2. temperatureThe mixture is refluxed for 11/2 hours
  3. filtrationfiltered while still hot
  4. customThe water is removed under vacuum
  5. customto give a semi-solid residue which
  6. customis triturated with hot isopropanol (3×100 ml.)
  7. customThe isopropanol is removed under vacuum
  8. customto give an oil which
  9. customis crystallized from isopropanol