反应详情

温度

80 °C

A mixture of 4-bromo-2-(2,6-dichloro-4-vinylphenyl)-7-fluoro-2H-pyrazolo[4,3-c]pyridine (295 mg, 0.76 mmol), 6-methylpyrimidin-4-ylamine (99 mg, 0.91 mmol), Pd2(dba)3 (17 mg, 0.019 mmol), Xantphos (44 mg, 0.076 mmol) and cesium carbonate (495 mg, 1.52 mmol) in dioxane (8.0 mL) was de-gassed and purged with nitrogen and the reaction mixture was heated at 80° C. in a sealed vial overnight. The resultant mixture was allowed to cool to room temperature, before being partitioned between ethyl acetate and water. The layers were separated and the organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (70-80% ethyl acetate in cyclohexane) to afford the title compound as a beige solid (197 mg, 62% yield). 1H NMR (400 MHz, DMSO-d6): δ 10.69 (s, 1H), 9.24 (d, J=2.6 Hz, 1H), 8.67 (d, J=1.2 Hz, 1H), 8.36 (s, 1H), 7.98-7.93 (m, 3H), 6.88-6.78 (m, 1H), 6.22 (d, J=17.6 Hz, 1H), 5.58 (d, J=11.0 Hz, 1H), 2.43 (s, 3H).

1. customwas de-gassed
2. custompurged with nitrogen
3. temperatureto cool to room temperature
4. custombefore being partitioned between ethyl acetate and water
5. customThe layers were separated
6. washthe organic layer was washed with brine
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified by silica gel flash chromatography (70-80% ethyl acetate in cyclohexane)