HRID357573

反应详情

EQUATION

反应方程式

HRID 357573 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

4.05 g (0.02 mol) of 4-methoxypropoxy-2-methylpyridine 1-oxide was dissolved in 50 ml of acetic anhydride to obtain a solution. This solution was stirred at 90° C. for 0.5 hour and cooled, followed by the addition of ethanol. The obtained mixture was concentrated under a reduced pressure, followed by the addition of 150 ml of 1N hydrochloric acid. The obtained mixture was stirred at 100° C. for one hour, cooled, neutralized with sodium hydrogencarbonate and, extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was distilled to remove the solvent. Thus, 3.64 g of the title compound was obtained as a crude product.

WORKUP

后处理

  1. customto obtain a solution
  2. temperaturecooled
  3. concentrationThe obtained mixture was concentrated under a reduced pressure
  4. additionfollowed by the addition of 150 ml of 1N hydrochloric acid
  5. stirringThe obtained mixture was stirred at 100° C. for one hour
  6. temperaturecooled
  7. extractionextracted with chloroform
  8. dry with materialThe extract was dried over magnesium sulfate
  9. filtrationfiltered
  10. distillationThe filtrate was distilled
  11. customto remove the solvent