반응 #1607443

반응 방정식

4-((1-(4-(5-ethylpyrimidin-2-yl)-2-methylphenyl)-4,4,4-trifluorobutyl)amino)benzoic acid

ethyl (3R)-piperidine-3-carboxylate

1-hydroxybenzotriazole

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride

diisopropylethylamine

→

title compound

ethyl (3R)-1-(4-((1-(4-(5-ethylpyrimidin-2-yl)-2-methylphenyl)-4,4,4-trifluorobutyl)amino)benzoyl)piperidine-3-carboxylate

용매

water

dimethylformamide

반응 조건

후처리

1. 1
   추출the mixture was extracted with ethyl acetate
2. 2
   세척The extract was washed with water and saturated brine
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   기타The solvent was evaporated under reduced pressure
5. 5
   기타the residue was purified by silica gel column chromatography (hexane/ethyl acetate)

실험 절차

A solution of 4-((1-(4-(5-ethylpyrimidin-2-yl)-2-methylphenyl)-4,4,4-trifluorobutyl)amino)benzoic acid obtained in step B, ethyl (3R)-piperidine-3-carboxylate (5.08 mL), 1-hydroxybenzotriazole (4.46 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (6.32 g) and diisopropylethylamine (5.76 mL) in dimethylformamide (79 mL) was stirred at room temperature overnight. The reaction mixture was added to water, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (15.9 g).

출처