HRID4629

反应详情

EQUATION

反应方程式

HRID 4629 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.33 g (2 mmol) of benzoyl isothiocyanate are added to 0.68 g (2 mmol) of N-[2-hydroxy-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-hydrazine carbothioamide in 20 ml of THF and the reaction mixture is stirred overnight at room temperature. After removal of the THF by evaporation, the solid residue is washed with ether and dissolved in 30 ml of ethanol with heating, and 1 ml of 30% hydrogen peroxide is added. The sulphur which separates is filtered off, the filtrate is concentrated by evaporation and the oily residue is purified by preparative layer chromotography.

WORKUP

后处理

  1. customAfter removal of the THF
  2. customby evaporation
  3. washthe solid residue is washed with ether
  4. dissolutiondissolved in 30 ml of ethanol
  5. temperaturewith heating
  6. addition1 ml of 30% hydrogen peroxide is added
  7. filtrationThe sulphur which separates is filtered off
  8. concentrationthe filtrate is concentrated by evaporation
  9. customthe oily residue is purified by preparative layer chromotography