반응 #157778

반응 방정식

1-Hydroxybenzotriazole

N,N-diethylethylenediamine

1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride

4-[(E)-2-cyclopentyl-1-(5-cyclopropyl-6-oxo-1,6-dihydropyridin-2-yl)ethenyl]benzoic acid

→

title compound

수율 26.0%

4-[(E)-2-Cyclopentyl-1-(5-cyclopropyl-6-oxo-1,6-dihydropyridin-2-yl)ethenyl]-N-[2-(diethylamino)ethyl]benzamide

수율 26.0%

용매

Water

N,N-dimethylformamide

triethylamine

반응 조건

후처리

1. 1
   추출followed by extraction with ethyl acetate
2. 2
   건조The organic layer was dried over anhydrous magnesium sulfate
3. 3
   여과filtered
4. 4
   기타The solvent was then evaporated under reduced pressure
5. 5
   기타The resulting residue was purified by preparative TLC (chloroform:methanol=20:1)
6. 6
   세척the resulting solid was washed with diethyl ether

실험 절차

1-Hydroxybenzotriazole (39 mg), triethylamine (0.04 mL), N,N-diethylethylenediamine (0.061 mL) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (55 mg) were sequentially added to a solution of 4-[(E)-2-cyclopentyl-1-(5-cyclopropyl-6-oxo-1,6-dihydropyridin-2-yl)ethenyl]benzoic acid (50 mg) in N,N-dimethylformamide at room temperature, and the mixture was stirred at room temperature overnight. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The resulting residue was purified by preparative TLC (chloroform:methanol=20:1) and the resulting solid was washed with diethyl ether to give the title compound as a white solid (17 mg, 26%).

출처