反应详情

A suspension of 4-bromo-7-chloro-2-(2,6-dichlorophenyl)-2H-pyrazolo[4,3-c]pyridine (200 mg, 0.53 mmol), (6-amino-pyrimidin-4-yl)-methanol (73 mg, 0.58 mmol), Pd2(dba)3 (24 mg, 0.025 mmol), Xantphos (31 mg, 0.05 mmol) and cesium carbonate (347 mg, 1.1 mmol) in dioxane (3 mL) was sealed in a microwave vial, purged with nitrogen, and irradiated in a microwave reactor at 150° C. for 30 min. 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 NH2 silica gel flash chromatography (0-2% methanol in ethyl acetate), to afford the title compound as a pale yellow solid (57 mg, 34% yield). 1H (400 MHz, DMSO-d6+d-TFA): δ 9.36 (s, 1H), 9.04 (s, 1H), 8.27 (bs, 1H), 8.16 (s, 1H), 7.80 (d, J=1.2 Hz, 1H), 7.78 (s, 1H), 7.70 (dd, J=9.0, 7.3 Hz, 1H), 4.67 (s, 2H). LCMS (Method B): RT=3.19 min, m/z: 421 [M+H+].

1. customwas sealed in a microwave vial
2. custompurged with nitrogen
3. customirradiated in a microwave reactor at 150° C. for 30 min
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 NH2 silica gel flash chromatography (0-2% methanol in ethyl acetate)