HRID65036

反应详情

EQUATION

反应方程式

HRID 65036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 50 ml of acetonitrile was dissolved 2.3 g of N-methylbenzoylaminothioacetamide. In the solution was suspended 4.0 g of 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide. To the suspension was added while stirring 1.5 ml of triethylamine, followed by further stirring under reflux. The reaction solution was left standing for cooling, then the solvent was evaporated off. To the residue was added a saturated aqueous solution of sodium hydrogen carbonate. The mixture was subjected to extraction with ethyl acetate. The extract solution was washed with water, dried, then, the solvent was evaporated off. The residue was purified by means of a silica-gel column chromatography (eluent: ethyl acetate) to give 3.2 g (yield 72%) of 2-(N-methylbenzoylaminomethyl)-4-(4-methoxyphenyl)-5-(3-pyridyl)-1,3-thiazole.

WORKUP

后处理

  1. additionTo the suspension was added
  2. temperatureunder reflux
  3. waitThe reaction solution was left
  4. temperaturefor cooling
  5. customthe solvent was evaporated off
  6. additionTo the residue was added a saturated aqueous solution of sodium hydrogen carbonate
  7. extractionThe mixture was subjected to extraction with ethyl acetate
  8. washThe extract solution was washed with water
  9. customdried
  10. customthe solvent was evaporated off
  11. customThe residue was purified by means of a silica-gel column chromatography (eluent: ethyl acetate)