반응 #2609

반응 방정식

ammonium chloride

sodium hydride

4-Acetylamino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(4-methoxyphenyl)benzamide

methyl iodide

→

title compound

수율 80.4%

4-(N-Methylacetylamino)-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(4-methoxyphenyl)benzamide

수율 80.4%

용매

THF

반응 조건

후처리

1. 1
   기타at room temperature
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The resulting organic layer was washed with water and saturated brine
4. 4
   건조dried on anhydrous sodium sulfate
5. 5
   기타Thereafter, the solvent was removed by evaporation
6. 6
   기타the resulting residue was recrystallized from methanol-ether

실험 절차

4-Acetylamino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(4-methoxyphenyl)benzamide (155.0 mg, 0.30 mmol) was dissolved in THF (3.0 ml) to which were subsequently added 60% sodium hydride {28.0 mg, 0.70 mmol) and methyl iodide (0.060 ml, 1.00 mmol) at room temperature, followed by 2 hours of stirring. The reaction solution was mixed with saturated ammonium chloride aqueous solution and extracted with ethyl acetate. The resulting organic layer was washed with water and saturated brine, and dried on anhydrous sodium sulfate. Thereafter, the solvent was removed by evaporation, and the resulting residue was recrystallized from methanol-ether to obtain 128.0 mg (80.4%) of the title compound in a colorless powder form.

출처