HRID847124

反应详情

EQUATION

反应方程式

HRID 847124 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 g of 2,3-dichloropyridine, 11.2 g of anhydrous potassium carbonate and 100 ml of dimethylsulfoxide were mixed to obtain a suspension. To this suspension, 10 ml of a dimethylsulfoxide solution of 10.1 g of benzyl mercaptan was dropwise added over a period of about 20 minutes at 110° C. Then, the mixture was reacted at a temperature of from 120 to 130° C. for about 1.5 hours. Thereafter, the reaction product was put into water and extracted with methylene chloride. The methylene chloride layer was dried over anhydrous sodium sulfate. Then, methylene chloride was distilled off under reduced pressure, and the obtained residue was purified by silica gel column chromatography to obtain 12.5 g of oily 2-benzylthio-3-chloropyridine.

WORKUP

后处理

  1. customto obtain a suspension
  2. customThen, the mixture was reacted at a temperature of from 120 to 130° C. for about 1.5 hours
  3. extractionextracted with methylene chloride
  4. dry with materialThe methylene chloride layer was dried over anhydrous sodium sulfate
  5. distillationThen, methylene chloride was distilled off under reduced pressure
  6. customthe obtained residue was purified by silica gel column chromatography