HRID1395402
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 solution of 34.6 g. of ethyl α-acetamido-β-oxo-γ-bromobutyrate in a mixture of 50 ml. of ethanol and 20 ml. of ether are added 18.9 g. of N-acetylthiourea and 15 ml. of pyridine. The mixture is heated under reflux for 4 hours, and condensed under reduced pressure. The condensate is extracted with ethyl acetate and the extract is washed with 5% aq. NaHCO3, then with water, and dried. The oily substance which is obtained from the extract by removal of the solvent is purified by silica gel chromatography to give ethyl α-acetamido-2-acetamidothiazol-4-ylacetate. 4.46 g. Melting point: 148.9°-150° C.
WORKUP
后处理
- temperatureThe mixture is heated
- temperatureunder reflux for 4 hours
- customcondensed under reduced pressure
- extractionThe condensate is extracted with ethyl acetate
- washthe extract is washed with 5% aq. NaHCO3
- dry with materialwith water, and dried
- customThe oily substance which is obtained from the
- extractionextract by removal of the solvent
- customis purified by silica gel chromatography