반응 #2610

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

2,5-dimethoxytetrahydrofuran

→

title compound

수율 82.6%

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

수율 82.6%

용매

acetic acid

반응 조건

후처리

1. 1
   온도heated for 1 hour
2. 2
   온도under reflux
3. 3
   온도After 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
   세척the organic layer was washed with water and saturated brine
7. 7
   건조dried on anhydrous sodium sulfate
8. 8
   workup.DISTILLATIONThereafter, the solvent was distilled off under a reduced pressure
9. 9
   기타the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:4)

실험 절차

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.

출처