反应详情

To a solution of 4-[2-(3-bromophenyl)-6-(trifluoromethyl)pyrazolo[1,5-a]pyridin-3-yl]-N-(3-fluorophenyl)-2-pyrimidinamine (125 mg, 0.24 mmol) in dioxane (10 mL) was added Pd2 dba3 (7 mg, 0.007 mmol), Cs2CO3 (94 mg, 0.34 mmol), Xantphos (7 mg, 0.011 mmol), and 2,6-difluorobenzamide (44 mg, 0.28 mmol). The reaction mixture was then subjected to microwave irradiation (Personal Chemistry Optimizer, 170° C., 15 min). The reaction was then cooled and the mixture partitioned in EtOAc (100 mL) and water (25 mL). The organic layer was separated, dried (over MgSO4) and concentrated. The crude material was purified by silica gel column chromatography (20-50% EA/Hex) to provide the title compound (43 mg, 30%) as an beige solid. 1H NMR (400 MHz, d6-DMSO): δ 10.95 (s, 1H), 9.88 (s, 1H), 9.54 (s, 1H), 8.54 (d, J=9.3 Hz, 1H), 8.38 (d, J=5.3 Hz, 1H), 8.07 (s, 1H), 7.80 (d, J=8.8 Hz, 1H), 7.71 (m, 2H), 7.59 (m, 1H), 7.49 (t, J=8.0 Hz, 1H), 7.43 (d, J=9.3 Hz, 1H), 7.35 (d, J=7.7 Hz, 1H), 7.25 (m, 3H), 6.71 (dt, J=2.3, 8.4 Hz, 1H), 6.65 (d, J=5.1 Hz, 1H) ppm. ESIMS (M+H)+=605.

1. customThe reaction mixture was then subjected to microwave irradiation (Personal Chemistry Optimizer, 170° C., 15 min)
2. temperatureThe reaction was then cooled
3. customthe mixture partitioned in EtOAc (100 mL)
4. customThe organic layer was separated
5. dry with materialdried (over MgSO4)
6. concentrationconcentrated
7. customThe crude material was purified by silica gel column chromatography (20-50% EA/Hex)