反応 #2610

反応方程式

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

2,5-dimethoxytetrahydrofuran

→

title compound

収率 82.6%

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

収率 82.6%

溶媒

acetic acid

反応条件

後処理

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
   洗浄the organic layer was washed with water and saturated brine
7. 7
   乾燥dried on anhydrous sodium sulfate
8. 8
   workup.DISTILLATIONThereafter, the solvent was distilled off under a reduced pressure
9. 9
   その他the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:4)

実験手順

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.

出典