HRID450102

反应详情

EQUATION

反应方程式

HRID 450102 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of thiobenzamide (1 g, 7.3 mmol) in THF (10 ml) was added a solution of 2-bromo-1,1-diethoxy-ethane (1.4 g, 7.3 mmol) in THF (5 ml) and the reaction was heated at reflux overnight. The reaction mixture was cooled to room temperature and diluted with water (50 ml). The solution was basified with dilute sodium hydroxide and extracted with ethyl acetate: pet ether (1:4). The organic layer was then washed with water, brine and dried. Evaporation gave a residue which was purified by column chromatography over silica gel using EtOAc/pet ether as eluent to give 2-phenyl thiazole (400 mg, 34%) as solid.

WORKUP

后处理

  1. temperaturethe reaction was heated
  2. temperatureat reflux overnight
  3. extractionextracted with ethyl acetate: pet ether (1:4)
  4. washThe organic layer was then washed with water, brine
  5. customdried
  6. customEvaporation
  7. customgave a residue which
  8. customwas purified by column chromatography over silica gel