反应详情

温度

80 °C

3-Iodo-1-methyl-1H-pyrazolo[3,4-d]pyrimidin-4-ol (C8) (9.35 g, 33.9 mmol), N,N-dimethylformamide (10.5 mL, 135 mmol) and phosphorus oxychloride (9.57 mL, 102 mmol) were combined in 1,2-dichloroethane (90 mL), and the mixture was heated to 80° C. for 2 hours. After cooling to room temperature, it was added portion-wise with vigorous stirring to a beaker containing a chilled mixture (0 to 5° C.) of sodium bicarbonate (28.7 g, 339 mmol) in 2-propanol (90 mL) and water (90 mL). The resulting mixture was stirred at 0 to 5° C. for 6 hours, and then concentrated in vacuo. The resulting solid was collected via filtration, and washed with water to provide the product as a yellow solid. Yield: 8.45 g, 28.7 mmol, 85%. 1H NMR (500 MHz, DMSO-d6) δ 4.04 (s, 3H), 8.82 (s, 1H).

1. temperatureAfter cooling to room temperature
2. additionit was added portion-wise
3. stirringThe resulting mixture was stirred at 0 to 5° C. for 6 hours
4. concentrationconcentrated in vacuo
5. filtrationThe resulting solid was collected via filtration
6. washwashed with water