تفاعل #2610

معادلة التفاعل

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

2,5-dimethoxytetrahydrofuran

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title compound

المردود 82.6%

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

المردود 82.6%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated for 1 hour
2. 2
   درجة الحرارةunder reflux
3. 3
   درجة الحرارةAfter 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
   غسيلthe organic layer was washed with water and saturated brine
7. 7
   تجفيفdried on anhydrous sodium sulfate
8. 8
   workup.DISTILLATIONThereafter, the solvent was distilled off under a reduced pressure
9. 9
   أخرىthe resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:4)

الإجراء التجريبي

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.

المصدر