Reaktion #1005947
ord-287538803f06481ea775b8ec999614cc
Reaktionsgleichung
Ethyl 2-chloro-4-(trifluoromethyl)pyrimidine-5-carboxylate
3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidine
potassium carbonate
→
title compound
Ausbeute 95.0%
ethyl 2-[3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-4-(trifluoromethyl)pyrimidine-5-carboxylate
Ausbeute 95.0%
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling
- 2Extraktionextracted with ethyl acetate
- 3TrocknenThe organic layer was dried over magnesium sulfate
- 4SonstigeThe solvent was evaporated off under reduced pressure
- 5Sonstigethe residue was then purified by a silica gel chromatography
Vorschrift
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%).