反应详情

温度

100 °C

Phosphoryl trichloride (7.59 mL, 79.2 mmol) was added to 1-(3-methylpyridin-4-yl)-7H-pyrazolo[4,5-e]pyrimidin-4-one (Intermediate M2) (900 mg, 3.96 mmol) and the resulting suspension was stirred at 100° C. for 24 hours during which a solution formed. This was evaporated, triturated with ether (3×10 mL) and dried in vacuo. The resulting solid was suspended in DCM (50 mL) and stirred with 10 g of polymer supported carbonate for 2 hours. The mixture was filtered and evaporated to afford 4-chloro-1-(3-methylpyridin-4-yl)pyrazolo[5,4-d]pyrimidine (700 mg, 72%). 1H NMR (400 MHz, DMSO-d6) δ 2.25 (3H, s), 7.62 (1H, d), 8.64 (1H, d), 8.74 (1H, s), 8.83 (1H, s), 8.94 (1H, s); m/z (ESI+) (M+H)+=246; HPLC tR=1.22 min.

1. customformed
2. customThis was evaporated
3. customtriturated with ether (3×10 mL)
4. customdried in vacuo
5. stirringstirred with 10 g of polymer
6. customfor 2 hours
7. filtrationThe mixture was filtered
8. customevaporated