反应详情

温度

100 °C

Phosphorus oxychloride (7.76 mL, 83.24 mmol) was added to 1-(2,5-dimethylphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol (1 g, 4.16 mmol). The resulting solution was stirred at 100° C. for 2 hours. LCMS showed reaction was complete. The reaction mixture was evaporated. Ice/water and then EtOAc were added. The organic layer was separated and the aqueous layer re-extracted with EtOAc. The combined organics were washed with water, dried (MgSO4) and concentrated to give crude product (1.077 g, 100%) which was used without purification. 1H NMR (400 MHz, DMSO) δ 2.00 (3H, s), 2.35 (3H, s), 7.26-7.37 (3H, m), 8.72 (1H, s), 8.86 (1H, s); m/z (ES+) (M+H)+=259; HPLC tR=2.48 min.

1. customreaction
2. customThe reaction mixture was evaporated
3. additionIce/water and then EtOAc were added
4. customThe organic layer was separated
5. extractionthe aqueous layer re-extracted with EtOAc
6. washThe combined organics were washed with water
7. dry with materialdried (MgSO4)
8. concentrationconcentrated