HRID2107320

反应详情

EQUATION

反应方程式

HRID 2107320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 50 ml of acetone was dissolved 2.0 g of 2-mercaptoquinoxaline. To the solution were added 2.02 g of 2-picolyl chloride hydrochloride, 4.0 g of potassium carbonate and 5 ml of water. The resulting mixture was stirred at room temperature for 0.5 hr., and the solvent was removed under reduced pressure. The residue was extracted with chloroform after addition of chloroform and water. The organic layer was separated and dried over sodium sulfate. The sodium sulfate was removed by filtration, and the filtrate was placed under reduced pressure to remove the solvent. To the residue were added 20 ml of ethanol and 1.03 ml of conc. hydrchloric acid and then added ether. Thus precipitated crystals were washed with ethanol-ether (1:1) and dried under reduced pressure to give 2.09 g of 2-(2-pyridylmethylthio)quinoxaline hydrochloride as a yellow crystalline powder.

WORKUP

后处理

  1. custom, and the solvent was removed under reduced pressure
  2. extractionThe residue was extracted with chloroform
  3. additionafter addition of chloroform and water
  4. customThe organic layer was separated
  5. dry with materialdried over sodium sulfate
  6. customThe sodium sulfate was removed by filtration
  7. customto remove the solvent
  8. additionTo the residue were added 20 ml of ethanol and 1.03 ml of conc. hydrchloric acid
  9. washThus precipitated crystals were washed with ethanol-ether (1:1)
  10. customdried under reduced pressure