反应详情

温度

100 °C

Phosphorus oxychloride (8.90 mL, 95.52 mmol) was added to 3-(4-hydroxy-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-4-methylbenzonitrile (Intermediate AM3) (1.2 g, 4.78 mmol). The resulting solution was stirred at 100° C. for 4 hours. The reaction mixture was evaporated and then azetroped with toluene to remove any residual POCl3. Ice/water was added and the formed precipitate was filtered washing well with water and dried overnight in vacuo over P2O5 to afford 3-(4-chloro-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-4-methylbenzonitrile (1.16 g, 90%). 1H NMR (400 MHz, DMSO) 2.21 (3H, s), 7.73 (1H, d), 7.97-8.00 (1H, m), 8.06 (1H, d), 8.81 (1H, s), 8.91 (1H, s); HPLC tR=2.05 min.

1. customThe reaction mixture was evaporated
2. customto remove any residual POCl3
3. additionIce/water was added
4. filtrationthe formed precipitate was filtered
5. washwashing well with water
6. dry with materialdried overnight in vacuo over P2O5