HRID609851

反应详情

EQUATION

反应方程式

HRID 609851 反应方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

5.06 g (0.024 mol) of 4-(4-methoxybutoxy)-2-methylpyridine 1-oxide was dissolved in 80 ml of acetic anhydride to obtain a solution. This solution was stirred at 100° C. for one hour, cooled and distilled to remove the solvent. 150 ml of 1N hydrochloric acid was added to the residue. The obtained mixture was stirred at 100° C. for one hour, cooled, neutralized with sodium hydrogencarbonate and extracted with 200 ml of chloroform twice. The extract was dried over magnesium sulfate and filtered. The filtrate was distilled to remove the solvent and the residue was dried in a vacuum to obtain 5.66 g of the title compound as a crude oil.

WORKUP

后处理

  1. customto obtain a solution
  2. temperaturecooled
  3. distillationdistilled
  4. customto remove the solvent
  5. addition150 ml of 1N hydrochloric acid was added to the residue
  6. stirringThe obtained mixture was stirred at 100° C. for one hour
  7. temperaturecooled
  8. extractionextracted with 200 ml of chloroform twice
  9. dry with materialThe extract was dried over magnesium sulfate
  10. filtrationfiltered
  11. distillationThe filtrate was distilled
  12. customto remove the solvent
  13. customthe residue was dried in a vacuum