HRID67776

反应详情

EQUATION

反应方程式

HRID 67776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.6 g (0.02 mole) of 4-(4-chloro-3-chlorosulfonylphenyl)-2-(4-methoxyphenyl-imino)-3-methylthiazolidin-4-ol hydrobromide are introduced into a mixture of 10 ml of 40% strength aqueous methylamine and 150 ml of methanol and the resulting mixture is stirred for 20 hours at room temperature. The solvent is distilled off, the residue is taken up in 100 ml of ethanol and this solution is acidified with methanolic or ethanolic hydrogen chloride solution and heated at the boil for 2 hours. The solvent is distilled off, the residue is crystallized under ether, ethyl acetate or diisopropyl ether and the crystals are filtered off. Melting point 257° C. (with decomposition) (from isopropanol).

WORKUP

后处理

  1. distillationThe solvent is distilled off
  2. temperatureheated at the boil for 2 hours
  3. distillationThe solvent is distilled off
  4. customthe residue is crystallized under ether
  5. filtrationethyl acetate or diisopropyl ether and the crystals are filtered off