反应详情

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

1. extractionthe mixture was extracted with chloroform (3.0 L×4)
2. customThe organic layer obtained
3. concentrationwas concentrated until crystal
4. customprecipitated
5. additionTo the precipitate, n-hexane (2.5 L) was added
6. stirringThe resultant mixture was stirred under ice-
7. temperaturecool overnight The resultant solid
8. filtrationwas filtrated