反应 #2610

反应方程式

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

2,5-dimethoxytetrahydrofuran

→

title compound

收率 82.6%

4-(Pyrrole-1-yl)-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(4-methoxyphenyl)benzamide

收率 82.6%

溶剂

acetic acid

反应条件

后处理

1. 1
   温度heated for 1 hour
2. 2
   温度under reflux
3. 3
   温度After cooling
4. 4
   workup.DISTILLATIONacetic acid was distilled off under a reduced pressure
5. 5
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
6. 6
   洗涤the organic layer was washed with water and saturated brine
7. 7
   干燥dried on anhydrous sodium sulfate
8. 8
   workup.DISTILLATIONThereafter, the solvent was distilled off under a reduced pressure
9. 9
   其他the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:4)

实验过程

4-Amino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(4-methoxyphenyl)benzamide (237.0 mg, 0.50 mmol) was dissolved in acetic acid (5.0 ml), and the solution was mixed with 2,5-dimethoxytetrahydrofuran (0.065 ml, 0.50 mmol) and heated for 1 hour under reflux. After cooling, acetic acid was distilled off under a reduced pressure, the residue was dissolved in ethyl acetate, and the organic layer was washed with water and saturated brine, and dried on anhydrous sodium sulfate. Thereafter, the solvent was distilled off under a reduced pressure, and the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:4) to obtain 217.0 mg (82,7%) of the title compound in a colorless amorphous form.

来源