反应详情

温度

100 °C

A solution of 3-bromo-5-fluoro-1-trityl-pyrazolo[3,4-b]pyridine, 44, (16.86 g, 36.79 mmol), KOAc (10.83 g, 110.4 mmol) and 4,4,5,5-tetramethyl-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,3,2-dioxaborolane (14.01 g, 55.18 mmol) in DMF (250 mL) was degassed under a nitrogen stream for 40 min. To the mixture was added Pd(dppf)2Cl2 (3.00 g, 3.68 mmol). The reaction mixture was heated at 100° C. for 90 minutes. The reaction mixture was filtered through a pad of florisil and celite. The filtrate was diluted with ether and brine. The organic phase was dried over MgSO4, filtered and concentrated in vacuo. The product was dried on high vacuum pump 3 days. To the product was added 200 mL Et2O and the mixture was stirred and filtered. The filtrate was concentrated in vacuo. The crude residue was diluted with 150 mL hexanes and the suspension was stirred for 3 hours, filtered and concentrated in vacuo to afford 12.6 g of desired product.

1. filtrationThe reaction mixture was filtered through a pad of florisil and celite
2. additionThe filtrate was diluted with ether and brine
3. dry with materialThe organic phase was dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe product was dried on high vacuum pump 3 days
7. additionTo the product was added 200 mL Et2O
8. filtrationfiltered
9. concentrationThe filtrate was concentrated in vacuo
10. additionThe crude residue was diluted with 150 mL hexanes
11. stirringthe suspension was stirred for 3 hours
12. filtrationfiltered
13. concentrationconcentrated in vacuo