HRID1395402

反应详情

EQUATION

反应方程式

HRID 1395402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 4 hours
  3. customcondensed under reduced pressure
  4. extractionThe condensate is extracted with ethyl acetate
  5. washthe extract is washed with 5% aq. NaHCO3
  6. dry with materialwith water, and dried
  7. customThe oily substance which is obtained from the
  8. extractionextract by removal of the solvent
  9. customis purified by silica gel chromatography