反应详情

温度

90 °C

A suspension of 3,5-dichloro-4-(4,7-dibromo-pyrazolo[4,3-c]pyridin-2-yl)-benzonitrile (70 mg, 0.16 mmol), 6-methylpyrimidin-4-ylamine (18 mg, 0.17 mmol), Pd2(dba)3 (7 mg, 0.008 mmol), Xantphos (9 mg, 0.016 mmol) and cesium carbonate (104 mg, 0.31 mmol) in dioxane (3 mL) was sealed in a microwave vial, purged with nitrogen, and heated at 90° C. for 3.5 hours. The reaction mixture was cooled and partitioned between ethyl acetate and water. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resultant residue was purified by silica gel flash chromatography (0-100% ethyl acetate in cyclohexane), then futher triturated with diethyl ether then ethyl acetate to afford the title compound as a white solid (42 mg, 57% yield). 1H NMR (400 MHz, DMSO-d6): δ 10.90 (s, 1H), 9.35 (s, 1H), 8.71 (d, J=1.2 Hz, 1H), 8.50 (s, 2H), 8.37 (s, 1H), 8.17 (s, 1H), 2.45 (s, 3H). LCMS (Method B): RT=3.75 min, m/z: 476 [M+H+].

1. customwas sealed in a microwave vial
2. custompurged with nitrogen
3. temperatureThe reaction mixture was cooled
4. custompartitioned between ethyl acetate and water
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe resultant residue was purified by silica gel flash chromatography (0-100% ethyl acetate in cyclohexane)
8. customfuther triturated with diethyl ether