反应详情

A suspension of 3,5-dichloro-4-(4,7-dichloropyrazolo[4,3-c]pyridin-2-yl)benzonitrile (70 mg, 0.20 mmol), 6-methylpyrimidin-4-ylamine (23 mg, 0.22 mmol), Pd2(dba)3 (9 mg, 0.01 mmol), Xantphos (12 mg, 0.02 mmol) and cesium carbonate (130 mg, 0.40 mmol) in dioxane (3 mL) was sealed in a microwave vial, purged with nitrogen and irradiated at 150° C. for 30 minutes in the microwave. 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 residue was purified by silica gel flash chromatography (0-80% ethyl acetate in pentane), then further triturated with ethyl acetate to afford the title compound as a yellow solid (37 mg, 43% yield). 1H NMR (400 MHz, DMSO-d6): δ 10.90 (s, 1H), 9.33 (s, 1H), 8.71 (d, J=1.2 Hz, 1H), 8.51 (s, 2H), 8.37 (s, 1H), 8.08 (s, 1H), 2.45 (s, 3H). LCMS (Method B): RT=3.69 min, m/z: 430 [M+H+].

1. customwas sealed in a microwave vial
2. custompurged with nitrogen
3. customirradiated at 150° C. for 30 minutes in the microwave
4. temperatureThe reaction mixture was cooled
5. custompartitioned between ethyl acetate and water
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by silica gel flash chromatography (0-80% ethyl acetate in pentane)
9. customfurther triturated with ethyl acetate