反応 #1148621

反応方程式

4-chloro-3-methoxy-2-methylpyridine

hydrogen peroxide water

→

4-chloro-3-methoxy-2-methylpyridine N-oxide

溶媒

acetic acid

反応条件

後処理

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

実験手順

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).

出典