반응 #84284

반응 방정식

water

2-bromo-1-(3-chloro-5-methoxypyridin-2-yl)ethanone

potassium phthalimide

potassium iodide

→

desired product

수율 16.8%

N-[2-(3-chloro-5-methoxypyridin-2-yl)-2-oxoethyl]phthalimide

수율 16.8%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타After completion of the reaction
2. 2
   온도to cool to room temperature
3. 3
   추출extracted with ethyl acetate (40 ml×1)
4. 4
   건조the resulting organic layer was dried over saturated aqueous sodium chloride
5. 5
   기타anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
6. 6
   기타The resulting residue was purified by silica gel column chromatography

실험 절차

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.

출처