反应 #2609

反应方程式

ammonium chloride

sodium hydride

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

methyl iodide

→

title compound

收率 80.4%

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

收率 80.4%

溶剂

THF

反应条件

后处理

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

实验过程

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.

来源