HRID1073064

反应详情

EQUATION

反应方程式

HRID 1073064 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 7-chloro-2,3-dihydro-4(lH)-quinolinone (20.0 g), pyridine (26 g) and dichloromethane (200 ml) was added dropwise 2-methyl-3-thienylcarbonyl chloride (26 g) at room temperature with stirring. The mixture was stirred under reflux for 4 hours. The reaction mixture was poured into 500 ml of water, then shaken with additional dichloromethane (1000 ml). The organic layer was washed once with 1 N HCl (100 ml), twice with water (200 ml each) and once with saturated aqueous NaCl solution, then dried over anhydrous sodium sulfate. Solvent was removed in vacuo and 7-chloro-2,3-dihydro-l-(2-methyl-3-thienylcarbonyl)-4(lH)-quinolinone (yield 28 g) was obtained as colorless oil.

WORKUP

后处理

  1. stirringThe mixture was stirred
  2. temperatureunder reflux for 4 hours
  3. washThe organic layer was washed once with 1 N HCl (100 ml), twice with water (200 ml each) and once with saturated aqueous NaCl solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. customSolvent was removed in vacuo