反応 #168876

反応方程式

sodium thiosulfate

urea peroxide

phthalic anhydride

3-chloro-4-methoxy-2,5-dimethylpyridine

→

title compound

収率 91.5%

3-Chloro-4-methoxy-2,5-dimethylpyridine 1-oxide

収率 91.5%

溶媒

chloroform

dichloromethane

反応条件

後処理

1. 1
   温度under cooling on ice
2. 2
   抽出The water layer was extracted with chloroform two times
3. 3
   乾燥The organic layer was dried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONthe solvent was then distilled away

実験手順

The above 3-chloro-4-methoxy-2,5-dimethylpyridine (181 mg) was dissolved in 5 ml of dichloromethane, and urea peroxide (169 mg) and phthalic anhydride (219 mg) were then added to the solution. The resulting mixture was stirred at room temperature for 2.5 hours. Thereafter, a saturated aqueous sodium thiosulfate solution was added to the reaction solution under cooling on ice, and the resulting mixture was then diluted with chloroform. The water layer was extracted with chloroform two times. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away, so as to obtain the title compound (181 mg) as a solid.

出典