反应详情

温度

120 °C

3-(1-(4-amino-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-1-yl)ethyl)-4-phenyl-1H-isochromen-1-one (Intermediate D2a, 60 mg, 0.118 mmol), 2-(tributylstannyl)pyrazine (0.072 mL, 0.236 mmol), Pd(PPh3)4, (13.61 mg, 0.012 mmol) and LiCl (4.99 mg, 0.118 mmol) were reacted in dioxane (1.2 mL), purged under argon and heated at 120° C. overnigth. The reaction was quenched by the addition of 1M HClaqueous (2 ml), and the solids collected by filtration. The solid crude was straightforward purified via reverse phase chromatography using a Biotage C18 30 g SNAP with a gradient of water and acetonitrile (prior to drying 5 mL of 2M HClaqueous was added). The resulting white solid was triturated in Et2O. to give (13.5 mg, 24.8%) the title compound.

1. custompurged under argon
2. customThe reaction was quenched by the addition of 1M HClaqueous (2 ml)
3. filtrationthe solids collected by filtration
4. customThe solid crude was straightforward purified via reverse phase chromatography
5. customto drying 5 mL of 2M HClaqueous
6. additionwas added)
7. customThe resulting white solid was triturated in Et2O