反应详情

A suspension of 4-chloro-2-(2,6-dichloro-4-fluorophenyl)-2H-pyrazolo[4,3-c]pyridine (70 mg, 0.22 mmol), 6-methylpyrimidin-4-ylamine (26 mg, 0.24 mmol), Pd2(dba)3 (10 mg, 0.011 mmol), Xantphos (12.8 mg, 0.022 mmol) and cesium carbonate (144 mg, 0.44 mmol) in dioxane (3 ml) was sealed in a microwave vial, purged with nitrogen and irradiated at 150° C. for 25 minutes 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 resultant residue was purified by silica gel flash chromatography (50-100% ethyl acetate in cyclohexane), then further triturated with diethyl ether:pentane (1:1) to afford the title compound as a yellow solid (53 mg, 62% yield). 1H NMR (400 MHz, DMSO-d6): δ 10.65 (br s, 1H), 9.15 (s, 1H), 8.70 (s, 1H), 8.51 (s, 1H), 8.00 (d, J=6.4 Hz, 1H), 7.93 (d, J=8.4 Hz, 2H), 7.23 (d, J=6.4 Hz, 1H), 2.46 (s, 3H). LCMS (Method B): RT=2.94 min, m/z: 389 [M+H+].

1. customwas sealed in a microwave vial
2. custompurged with nitrogen
3. customirradiated at 150° C. for 25 minutes 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 resultant residue was purified by silica gel flash chromatography (50-100% ethyl acetate in cyclohexane)
10. customfurther triturated with diethyl ether:pentane (1:1)