反応 #84317

反応方程式

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

ethoxyamine hydrochloride

→

desired product

収率 89.3%

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

収率 89.3%

溶媒

ethanol

反応条件

後処理

1. 1
   その他After completion of the reaction
2. 2
   その他the solvent was evaporated under reduced pressure
3. 3
   workup.ADDITIONthe resulting residue was mixed with 4 ml of water
4. 4
   抽出extracted with ethyl acetate (4 ml×2)
5. 5
   乾燥dried over saturated aqueous sodium chloride
6. 6
   その他anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
7. 7
   その他The residue was purified by silica gel column chromatography

実験手順

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.

出典