反应详情

温度

100 °C

Phosphoryl trichloride (16.09 mL, 172.63 mmol) was added in one portion to 1-(3-chloro-2-methylphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol (Intermediate AE6) (3.0 g, 11.51 mmol) and the resulting suspension was heated to 100° C. to give a solution and stirred for 4 hours. Evaporated, the residue poured into ice/water and stirred for 30 minutes. The solids were filtered, washed with water (4×20 mL), dissolved in ethyl acetate (100 mL), dried (MgSO4), filtered and evaporated to afford the product (2.8 g) which was used without further purification. 1H NMR (400 MHz, DMSO) δ 2.06 (3H, s), 7.41-7.54 (2H, m), 7.71-7.73 (1H, m), 8.79 (1H, s), 8.89 (1H, s); m/z (ESI+) (M+H)+=279; HPLC tR=2.59 min.

1. customto give a solution
2. customEvaporated
3. additionthe residue poured into ice/water
4. stirringstirred for 30 minutes
5. filtrationThe solids were filtered
6. washwashed with water (4×20 mL)
7. dissolutiondissolved in ethyl acetate (100 mL)
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. customevaporated