反应详情

温度

160 °C

1-(5-Bromo-2-methylphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol (Intermediate AM4) (1.38 g, 4.52 mmol), and zinc cyanide (0.478 g, 4.07 mmol) were dissolved in DMF (15 mL) and sealed into a microwave tube. The reaction mixture was evacuated and back flushed with nitrogen several times. 9,9-Dimethyl-4,5-bis(diphenylphosphino)xanthene (0.262 g, 0.45 mmol) and tris(dibenzylideneacetone)dipalladium(0) (0.207 g, 0.23 mmol) were added. The reaction was heated to 160° C. for 10 minutes in the microwave reactor and cooled to RT. The reaction mixture was diluted with EtOAc (100 mL) and water (50 mL) and then filtered. Solid was taken up in hot methanol, filtered and dried under vacuum to afford the product (0.99 g, 89%) which was used without further purification. 1H NMR (400 MHz, DMSO) 2.19 (3H, s), 7.67 (1H, d), 7.92-7.96 (2H, m), 8.10 (1H, s), 8.35 (1H, s), 12.38 (1H, s); m/z (ES−) (M−H)−=250; HPLC tR=1.23 min.

1. customsealed into a microwave tube
2. customThe reaction mixture was evacuated
3. customback flushed with nitrogen several times
4. temperaturecooled to RT
5. filtrationfiltered
6. filtrationfiltered
7. customdried under vacuum