反应 #665229

反应方程式

sodium sulfite

sodium carbonate

2,3,5-trimethylpyridine

acetic acid

hydrogen peroxide water

→

title compound

收率 94.5%

2,3,5-trimethylpyridine 1-oxide

收率 94.5%

溶剂

water

反应条件

后处理

1. 1
   workup.ADDITIONThis reaction mixed solution
2. 2
   萃取the resultant mixture was extracted with chloroform (3.0 L×4)
3. 3
   浓缩The resultant organic layer was concentrated until crystals
4. 4
   其他precipitated
5. 5
   workup.ADDITIONThe precipitate was charged with n-hexane (2.5 L)
6. 6
   过滤The obtained crystals were filtered

实验过程

2,3,5-trimethylpyridine (1.43 kg, 11.80 mol) was charged over 15 minutes into acetic acid (1.43 kg, 23.83 mol). After 15 minutes, 35% hydrogen peroxide water (1.38 kg, 14.2 mol) was added dropwise into the solution over 30 minutes. The resultant solution was then stirred overnight at 90 to 95° C. The reaction solution was charged with sodium sulfite (220 g). This reaction mixed solution was charged with sodium carbonate (2.5 kg) and water (12 L), and the resultant mixture was extracted with chloroform (3.0 L×4). The resultant organic layer was concentrated until crystals precipitated. The precipitate was charged with n-hexane (2.5 L), and the solution was stirred overnight under ice cooling. The obtained crystals were filtered to obtain 1.53 kg of the title compound.

来源