HRID325528
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
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
- additionTo this solution is added 18.1 g
- temperatureThe mixture is refluxed for 11/2 hours
- filtrationfiltered while still hot
- customThe water is removed under vacuum
- customto give a semi-solid residue which
- customis triturated with hot isopropanol (3×100 ml.)
- customThe isopropanol is removed under vacuum
- customto give an oil which
- customis crystallized from isopropanol