反应 #1005947

反应方程式

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

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

potassium carbonate

→

title compound

收率 95.0%

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

收率 95.0%

溶剂

N,N-dimethylformamide

反应条件

后处理

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

实验过程

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%).

来源