反应详情

A suspension of 4-bromo-2-(2,6-dichlorophenyl)-7-methoxy-2H-pyrazolo[4,3-c]pyridine (135 mg, 0.36 mmol), (6-aminopyrimidin-4-yl)methanol (50 mg, 0.4 mmol), Pd2(dba)3 (8 mg, 0.009 mmol), Xantphos (43 mg, 0.036 mmol) and cesium carbonate (235 mg, 0.72 mmol) in dioxane (3 mL) was sealed in a microwave vial, purged with nitrogen and irradiated at 150° C. for 1 hour in the microwave. The reaction mixture was cooled and partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (0-2% methanol in ethyl acetate) to afford the title compound as a yellow solid (62 mg, 41% yield). 1H NMR (400 MHz, DMSO-d6): δ 10.42 (s, 1H), 9.11 (s, 1H), 8.64 (d, J=0.9 Hz, 1H), 8.58 (d, J=1.2 Hz, 1H), 7.83 (d, J=1.3 Hz, 1H), 7.80 (s, 1H), 7.72 (dd, J=7.5, 9.2 Hz, 1H), 7.58 (s, 1H), 5.54 (t, J=6.0 Hz, 1H), 4.50 (d, J=6.0 Hz, 2H), 3.97 (s, 3H). LCMS (Method B): RT=2.75 min, m/z: 417 [M+H+].

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