Реакция #2610

Уравнение реакции

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

2,5-dimethoxytetrahydrofuran

→

title compound

Выход 82.6%

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

Выход 82.6%

Растворители

acetic acid

Условия реакции

Обработка

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

Методика

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.

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