反応 #2609

反応方程式

ammonium chloride

sodium hydride

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

methyl iodide

→

title compound

収率 80.4%

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

収率 80.4%

溶媒

THF

反応条件

後処理

1. 1
   その他at room temperature
2. 2
   抽出extracted with ethyl acetate
3. 3
   洗浄The resulting organic layer was washed with water and saturated brine
4. 4
   乾燥dried on anhydrous sodium sulfate
5. 5
   その他Thereafter, the solvent was removed by evaporation
6. 6
   その他the resulting residue was recrystallized from methanol-ether

実験手順

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.

出典