反应详情

温度

80 °C

To 570 mg of 2-bromo-1-(3-chloro-5-methoxypyridin-2-yl)ethanone in 10 ml of N,N-dimethylformamide, 800 mg of potassium phthalimide and 36 mg of potassium iodide were added, and the mixture was stirred at 80° C. for 5 hours. After completion of the reaction, the reaction mixture was allowed to cool to room temperature, mixed with 20 ml of water and extracted with ethyl acetate (40 ml×1), the resulting organic layer was dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:9 to 3:7) as the eluent to obtain 0.12 g of the desired product as white crystals.

1. customAfter completion of the reaction
2. temperatureto cool to room temperature
3. extractionextracted with ethyl acetate (40 ml×1)
4. dry with materialthe resulting organic layer was dried over saturated aqueous sodium chloride
5. customanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography