反应 #1148621

ord-33f6df645d154677aa5c5b80a33a661c

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.DISTILLATIONthe reaction solution was distilled off under reduced pressure
  2. 2
    workup.DISSOLUTIONThe resulting residue was dissolved in chloroform
  3. 3
    洗涤washed with saturated sodium bicarbonate solution, and saturated salt water
  4. 4
    干燥dried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

实验过程

36.98 g of 4-chloro-3-methoxy-2-methylpyridine (V) was dissolved in 685 ml of acetic acid and 92 ml of hydrogen peroxide water was added thereto and the resulting mixture was heated at 90° C. for 24 hours, and thereafter, the reaction solution was distilled off under reduced pressure. The resulting residue was dissolved in chloroform and washed with saturated sodium bicarbonate solution, and saturated salt water, and thereafter, dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 37.64 g of 4-chloro-3-methoxy-2-methylpyridine N-oxide (VI).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06525066B2uspto-grants-2003_02