반응 #84255

반응 방정식

2-bromo-1-(3,5-dichloropyridin-2-yl)ethanone

ethoxyamine hydrochloride

→

desired product

수율 87.1%

2-bromo-1-(3,5-dichloropyridin-2-yl)ethanone-O-ethyloxime

수율 87.1%

용매

ethanol

반응 조건

후처리

1. 1
   기타After completion of the reaction
2. 2
   기타the solvent was evaporated under reduced pressure
3. 3
   workup.ADDITIONthe resulting residue was mixed with 50 ml of water
4. 4
   추출extracted with ethyl acetate (50 ml×2)
5. 5
   세척washed with water (50 ml×1)
6. 6
   건조dried over saturated aqueous sodium chloride
7. 7
   기타anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
8. 8
   기타The resulting residue was purified by silica gel column chromatograph

실험 절차

To 3.00 g of 2-bromo-1-(3,5-dichloropyridin-2-yl)ethanone in 25 ml of ethanol, 1.09 g of ethoxyamine hydrochloride was added, and the mixture was stirred at room temperature for 16 hours. After completion of the reaction, the solvent was evaporated under reduced pressure, the resulting residue was mixed with 50 ml of water and extracted with ethyl acetate (50 ml×2), the resulting organic layers were combined, washed with water (50 ml×1) and 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 chromatograph using ethyl acetate-hexane (with a gradient of from 5:95 to 15:85) as the eluent to obtain 3.03 g of the desired product as a colorless oil.

출처