HRID461725
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 a stirred and refluxing solution of 3.06 parts of 2-amino-2-thiazoline in 60 parts of dioxane is added a solution of 4.2 parts of p-(2-thenoyl)hydratropoyl chloride in 45 parts of dioxane. Upon completion, stirring at reflux is continued for 30 minutes. The reaction mixture is cooled, filtered and the filtrate is evaporated. The residue is purified by column-chromatography over silicagel, using a mixture of chloroform and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from ethanol, yielding N-(2-thiazoline-2-yl)-p-(2-thenoyl)hydratropamide; mp. 186.4° C.
WORKUP
后处理
- stirringUpon completion, stirring
- temperatureat reflux
- temperatureThe reaction mixture is cooled
- filtrationfiltered
- customthe filtrate is evaporated
- customThe residue is purified by column-chromatography over silicagel
- additiona mixture of chloroform and 5% of methanol as eluent
- customThe pure fractions are collected
- customthe eluent is evaporated
- customThe residue is crystallized from ethanol