反应详情

3-Bromo-1-methyl-1H-pyrazolo[3,4-d]pyrimidin-6-ylamine (Intermediate 3) (0.33 g, 1.46 mmol) and 4-benzyloxy-3-fluoro phenylboronic acid (0.43 g, 1.75 mmol) are suspended in 1,4-dioxane (5 ml) in a microwave vial flushed with argon. A solution of Cs2CO3 (1.43 g, 4.38 mmol) in water (1.5 ml) is added followed by Pd(PPh3)4 (0.085 g, 0.073 mmol) and the reaction mixture is heated using microwave radiation at 150° C. for 0.5 hours. After cooling to room temperature the reaction mixture is diluted with EtOAc (100 ml) and washed with saturated NaHCO3. The organic portion is dried over MgSO4, filtered, concentrated in vacuo and the resulting crude solid is triturated with EtOAc (˜20 ml) to afford the title compound as an off-white solid.

1. customvial flushed with argon
2. temperaturethe reaction mixture is heated
3. customat 150° C.
4. customfor 0.5 hours
5. washwashed with saturated NaHCO3
6. dry with materialThe organic portion is dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customthe resulting crude solid is triturated with EtOAc (˜20 ml)