반응 #84317

반응 방정식

N-[2-(3,5-dibromopyridine-2-yl)-2-oxoethyl]-2-(trifluoromethyl)benzamide

ethoxyamine hydrochloride

→

desired product

수율 89.3%

N-[2-(3,5-dibromopyridine-2-yl)-2-(ethoxyimino)ethyl]-2-(trifluoromethyl)benzamide

수율 89.3%

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 4 ml of water
4. 4
   추출extracted with ethyl acetate (4 ml×2)
5. 5
   건조dried over saturated aqueous sodium chloride
6. 6
   기타anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
7. 7
   기타The residue was purified by silica gel column chromatography

실험 절차

To 200 mg of N-[2-(3,5-dibromopyridine-2-yl)-2-oxoethyl]-2-(trifluoromethyl)benzamide in 1.4 ml of ethanol, 63 mg of ethoxyamine hydrochloride was added, and the mixture was stirred at room temperature for 18 hours. After completion of the reaction, the solvent was evaporated under reduced pressure, the resulting residue was mixed with 4 ml of water and extracted with ethyl acetate (4 ml×2), the resulting organic layers were combined, dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 5:95 to 50:50) as the eluent to obtain 195 mg of the desired product as a pale yellow resinous substance.

출처