HRID1062617

反应详情

EQUATION

反应方程式

HRID 1062617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of N-methylthiourea (0.24 g) in acetonitrile (18 mL) was added 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide (1.0 g) and triethylamine (0.4 mL) was slowly added dropwise with stirring. After completion of dropwise addition, the mixture was stirred at a refluxing temperature for 3 h, and the solvent was evaporated. To the residue was added saturated aqueous sodium hydrogencarbonate and the mixture was extracted with ethyl acetate, and the extract was washed with water and dried, and the solvent was evaporated. The remaining crude crystals were recrystallized from ethyl acetate-isopropyl ether to give the title compound (0.65 g, yield 85%).

WORKUP

后处理

  1. additionwas slowly added dropwise
  2. additionAfter completion of dropwise addition
  3. stirringthe mixture was stirred at a refluxing temperature for 3 h
  4. customthe solvent was evaporated
  5. additionTo the residue was added saturated aqueous sodium hydrogencarbonate
  6. extractionthe mixture was extracted with ethyl acetate
  7. washthe extract was washed with water
  8. customdried
  9. customthe solvent was evaporated
  10. customThe remaining crude crystals were recrystallized from ethyl acetate-isopropyl ether