HRID1640387

反应详情

EQUATION

反应方程式

HRID 1640387 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.71 g (11.3 mmol) of cesium carbonate were added to 1.10 g (5.42 mmol) of 4-chloro-3-mercapto-2-methylbenzoic acid in 20 ml of acetonitrile. The reaction mixture was stirred at RT for 10 min, and 1.02 g (6.51 mmol) of iodoethane were then slowly added dropwise. The reaction mixture was then stirred at RT for 16 h. The solvent was then removed, and a mixture of 20 ml of methanol and 2 ml of 20% strength aqueous sodium hydroxide solution was then added to the reaction mixture. For the hydrolysis of the ethyl ester formed, the mixture was stirred at RT for 16 h and then freed from the solvents. The residue was taken up in water and acidified with diluted HCl, and the mixture was stirred at RT for 10 min and then filtered. The residue was washed with water and sucked dry. 1.15 g of clean product were isolated.

WORKUP

后处理

  1. stirringThe reaction mixture was then stirred at RT for 16 h
  2. customThe solvent was then removed
  3. additiona mixture of 20 ml of methanol and 2 ml of 20% strength aqueous sodium hydroxide solution
  4. additionwas then added to the reaction mixture
  5. customFor the hydrolysis of the ethyl ester
  6. customformed
  7. stirringthe mixture was stirred at RT for 16 h
  8. stirringthe mixture was stirred at RT for 10 min
  9. filtrationfiltered
  10. washThe residue was washed with water
  11. customsucked dry