反应详情

温度

80 °C

A mixture of 5-bromo-2,3-difluoropyridine (1.9 g, 9.79 mmol) and 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (2.038 g, 9.79 mmol), Na2CO3 (2.076 g, 19.59 mmol) and Pd(PPh3)4 (1.131 g, 0.979 mmol) in DMF (8 ml) was bubbled with N2 for 10 min and was then heated to 80° C. for 10 h. After being cooled to rt, the mixture was filtered and the filtrate was diluted with EA, washed with water and brine, dried over anhydrous MgSO4. Filtered and concentrated. The residue was purified by silica gel chromatography eluted with Hex/EA (from 100% to 20%) to afford the title compound as a white solid (1.5 g, 57.4% yield). 1H-NMR (400 MHz, DMSO-d6) δ ppm 8.29 (d, 3H), 7.99 (d, 1H), 3.87 (s, 3H). LCMS (method B): [M+H]+=196, tR=1.91 min.

1. customwas bubbled with N2 for 10 min
2. temperatureAfter being cooled to rt
3. filtrationthe mixture was filtered
4. additionthe filtrate was diluted with EA
5. washwashed with water and brine
6. dry with materialdried over anhydrous MgSO4
7. filtrationFiltered
8. concentrationconcentrated
9. customThe residue was purified by silica gel chromatography
10. washeluted with Hex/EA (from 100% to 20%)