反应详情

A microwave reaction vial was charged with 2-chloro-3-nitro-5-(trifluoromethyl)pyridine (2 g, 8.83 mmol), NMP (4.41 ml) and CuCN (0.830 g, 9.27 mmol). The vial was sealed and the mixture was irradiated in the MW at 175° C. for 15 min. Upon cooling to RT, the reaction mixture was poured onto ice and EtOAc was added. The mixture was filtered through Celite, washing with EtOAc and a small amount of MeOH. The layers of the filtrate were separated, and the aqueous portion was extracted again with EtOAc. The combined organic portions were dried with sodium sulfate, filtered and concentrated. The crude material was purified by silica gel chromatography, using a gradient of 0-30% EtOAc in heptane to provide 3-nitro-5-(trifluoromethyl)picolinonitrile (645 mg, 2.97 mmol, 33.7% yield) as a yellow oil that solidified upon standing. LC/MS (ESI) m/z=218.1 (M+H).

1. customA microwave reaction
2. customThe vial was sealed
3. customthe mixture was irradiated in the MW at 175° C. for 15 min
4. additionwas added
5. filtrationThe mixture was filtered through Celite
6. washwashing with EtOAc
7. customThe layers of the filtrate were separated
8. extractionthe aqueous portion was extracted again with EtOAc
9. dry with materialThe combined organic portions were dried with sodium sulfate
10. filtrationfiltered
11. concentrationconcentrated
12. customThe crude material was purified by silica gel chromatography