反応 #1005947

反応方程式

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

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

potassium carbonate

→

title compound

収率 95.0%

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

収率 95.0%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   温度After cooling
2. 2
   抽出extracted with ethyl acetate
3. 3
   乾燥The organic layer was dried over magnesium sulfate
4. 4
   その他The solvent was evaporated off under reduced pressure
5. 5
   その他the residue was then purified by a silica gel chromatography

実験手順

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%).

出典