反应详情

温度

120 °C

A mixture of piperazin-2-one (4.85 g, 48.47 mmol, Avocado Research), 2-chloro-3-trifluoromethyl-pyridine (8.8 g, 48.47 mmol, TCI America) and diisopropylethylamine (111 mL, 58.16 mmol, Aldrich) in DMSO (160 mL) was heated at 120° C. for 16 h. The mixture was cooled to room temperature, diluted with H2O (500 mL) and extracted with EtOAc (2×500 mL). The combined organic extracts were dried over MgSO4 and filtered. The solvent was removed in vacuo and the residue was purified by silica gel column chromatography, eluting with dichloromethane/MeOH (15:1) to give the title compound as a yellow solid. MS (ESI, positive ion) m/z: 206 (M+1).

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with EtOAc (2×500 mL)
3. dry with materialThe combined organic extracts were dried over MgSO4
4. filtrationfiltered
5. customThe solvent was removed in vacuo
6. customthe residue was purified by silica gel column chromatography
7. washeluting with dichloromethane/MeOH (15:1)