HRID884992

反应详情

EQUATION

反应方程式

HRID 884992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 10.0 g of 3-ethylpyridine, 60 ml of acetic acid and 12 ml of 30% hydrogen peroxide solution was stirred while heating at 80° C. for 2.5 hours. To the reaction mixture, 7 ml of 30% hydrogen peroxide solution was added, and the reaction mixture was stirred while heating at 80° C. for further seven hours. The reaction mixture was cooled to room temperature, and sodium carbonate was added to the reaction mixture in small portions. The reaction mixture was filtered, and washed with ethyl acetate. The resultant filtrate was washed with a saturated aqueous solution of sodium hydrogen sulfite and a saturated sodium chloride solution, dried over anhydrous water sodium carbonate. Activated carbon was added, followed by filtration through Celite™. The filtrate was concentrated under reduced pressure to give 6.0 g of 3-ethylpyridine N-oxide.

WORKUP

后处理

  1. stirringthe reaction mixture was stirred
  2. temperaturewhile heating at 80° C. for further seven hours
  3. temperatureThe reaction mixture was cooled to room temperature
  4. filtrationThe reaction mixture was filtered
  5. washwashed with ethyl acetate
  6. washThe resultant filtrate was washed with a saturated aqueous solution of sodium hydrogen sulfite
  7. dry with materiala saturated sodium chloride solution, dried over anhydrous water sodium carbonate
  8. additionActivated carbon was added
  9. filtrationfollowed by filtration through Celite™
  10. concentrationThe filtrate was concentrated under reduced pressure