HRID4629
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
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
- customAfter removal of the THF
- customby evaporation
- washthe solid residue is washed with ether
- dissolutiondissolved in 30 ml of ethanol
- temperaturewith heating
- addition1 ml of 30% hydrogen peroxide is added
- filtrationThe sulphur which separates is filtered off
- concentrationthe filtrate is concentrated by evaporation
- customthe oily residue is purified by preparative layer chromotography