HRID67779

反应详情

EQUATION

反应方程式

HRID 67779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.8 g (0.01 mole) of 4-(4-chloro-3-chlorosulfonylphenyl)-3-methyl-2-phenylimino-4-thiazoline hydrobromide are added in portions to a mixture of 5 ml (about 0.05 mole) of 40% strength aqueous dimethylamine solution and 50 ml of methanol (or ethanol), with external cooling and stirring, at a rate such that the temperature as far as possible does not rise above 35° C. The reaction mixture is stirred for 14 hours at room temperature, the solvent is distilled off under a waterpump vacuum and the residue is crystallized under 50 ml of water, stirring with a magnetic stirrer. Colorless crystals; melting point 178°-181° C.

WORKUP

后处理

  1. temperaturewith external cooling
  2. customas possible does not rise above 35° C
  3. stirringThe reaction mixture is stirred for 14 hours at room temperature
  4. distillationthe solvent is distilled off under a waterpump vacuum
  5. customthe residue is crystallized under 50 ml of water
  6. stirringstirring with a magnetic stirrer