반응 #2614

반응 방정식

sodium bicarbonate

pyridine

4-Amino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(3-pyridyl)benzamide

trifluoroacetic acid

→

title compound

수율 81.2%

4-Trifluoroacetylamino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(3-pyridyl)benzamide

수율 81.2%

용매

methylene chloride

반응 조건

후처리

1. 1
   기타at 0° C
2. 2
   추출extracted with chloroform
3. 3
   세척The resulting organic layer was washed with saturated sodium chloride aqueous solution and water in that order
4. 4
   건조dried on anhydrous sodium sulfate
5. 5
   기타Thereafter, the solvent was removed by evaporation
6. 6
   기타the resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1)

실험 절차

4-Amino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(3-pyridyl)benzamide (229.3 mg, 0.51 mmol) was dissolved in methylene chloride (2.0 ml) to which were subsequently added pyridine (0.05 ml, 0.62 mmol) and anhydrous trifluoroacetic acid (0.09 ml, 0.64 mmol) at 0° C. After 3 hours of stirring at 0° C. to room temperature, the reaction solution was mixed with saturated sodium bicarbonate aqueous solution and extracted with chloroform. The resulting organic layer was washed with saturated sodium chloride aqueous solution and water in that order, and dried on anhydrous sodium sulfate. Thereafter, the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain 224.8 mg (81.2%) of the title compound in a light yellow powder form.

출처