反应详情

温度

0 °C

2-Methyl-3-nitro-6-(pyrrolidin-3-yloxy)pyridine (1.3 g) was dissolved in dichloromethane (20 ml) and triethylamine (1.57 ml) was added. The solution was cooled to 0° C. and a solution of propionyl chloride (574 mg) in dichloromethane (5 ml) was added dropwise over 5 min. The reaction mixture was allowed to come to room temperature and was stirred for another 5 min. Water (10 ml) was added. After stirring for 3 min, the phases were separated and the aqueous layer was extracted with dichloromethane. The combined organic layers were dried (sodium sulfate) and concentrated in vacuo. The crude product was purified by flash chromatography (silica, dichloromethane/methanol=98/2). Yield: 950 mg (64.9%, pale yellow oil).

1. customto come to room temperature
2. stirringAfter stirring for 3 min
3. customthe phases were separated
4. extractionthe aqueous layer was extracted with dichloromethane
5. dry with materialThe combined organic layers were dried (sodium sulfate)
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by flash chromatography (silica, dichloromethane/methanol=98/2)