反应详情

温度

80 °C

4-(trifluoromethyl)phenylboronic acid (500 mg, 2.63 mmol), 2-chloro-5-nitropyridine (417 mg, 2.63 mmol), potassium carbonate (908 mg, 6.58 mmol) and palladium(II) acetate (23.6 mg, 0.105 mmol) were combined in 1:1 dioxane:water (10 mL). The resulting mixture was stirred at 80° C. for 12 hours. The mixture was filtered and the solution was extracted with ethyl acetate. The organic layer was washed with water, then brine, dried over sodium sulfate, filtered and concentrated. Purification by column chromatography gave 5-nitro-2-(4-(trifluoromethyl)phenyl)pyridine (260 mg, 37%). 1H NMR (400 MHz, CDCl3, δ): 9.47 (s, 1H), 8.51 (d, 1H), 8.14 (d, 2H), 7.72 (d, 1H), 7.65 (d, 2H).

1. filtrationThe mixture was filtered
2. extractionthe solution was extracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialbrine, dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by column chromatography