HRID2304605

反应详情

EQUATION

反应方程式

HRID 2304605 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 N-methylthiourea (484 mg) in acetonitrile (40 mL), was added 2-bromo-2-phenyl-1-(3-pyridyl)ethanone hydrobromide (2.0 g), and then triethylamine (0.8 mL) was added dropwise to the mixture with stirring. After addition, the resulting mixture was stirred at reflux for 3 h and the solvent was evaporated. An aqueous saturated solution of sodium hydrogen carbonate was added to the residue and extracted with ethyl acetate. The extracts were washed with water, dried and the solvent was evaporated. The crystalline residue was recrystallized from ethyl acetate-isopropyl ether to give the title compound (1.2 g, yield 80%).

WORKUP

后处理

  1. additionAfter addition
  2. stirringthe resulting mixture was stirred
  3. temperatureat reflux for 3 h
  4. customthe solvent was evaporated
  5. additionAn aqueous saturated solution of sodium hydrogen carbonate was added to the residue
  6. extractionextracted with ethyl acetate
  7. washThe extracts were washed with water
  8. customdried
  9. customthe solvent was evaporated
  10. customThe crystalline residue was recrystallized from ethyl acetate-isopropyl ether