반응 #1005947

반응 방정식

Ethyl 2-chloro-4-(trifluoromethyl)pyrimidine-5-carboxylate

3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidine

potassium carbonate

→

title compound

수율 95.0%

ethyl 2-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-4-(trifluoromethyl)pyrimidine-5-carboxylate

수율 95.0%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   추출extracted with ethyl acetate
3. 3
   건조The organic layer was dried over magnesium sulfate
4. 4
   기타The solvent was evaporated off under reduced pressure
5. 5
   기타the residue was then purified by a silica gel chromatography

실험 절차

Ethyl 2-chloro-4-(trifluoromethyl)pyrimidine-5-carboxylate (1.2 g) [see J. Med. Chem., 43, 3995 (2000)], 3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidine (1.5 g), and potassium carbonate (0.7 g) were added to N,N-dimethylformamide (50 mL) and the mixture was heated at 100° C. for 5 hours. After cooling, the reaction solution was poured over ice water, and then extracted with ethyl acetate. The organic layer was dried over magnesium sulfate. The solvent was evaporated off under reduced pressure, and the residue was then purified by a silica gel chromatography to obtain the title compound (2.4 g, 95%).

출처