HRID1167649

反应详情

EQUATION

反应方程式

HRID 1167649 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 (242 mg) in acetonitrile (18 mL), was added 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide (1.0 g) and then triethylamine (0.4 mL) was added slowly dropwise to the mixture. 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 afford the title compound (650 mg, yield 85%).

WORKUP

后处理

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