反应详情

To a suspension of 4,6-bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine (1.00 g, 2.6 mmol, obtained in example 1) in CHCl3 (10 mL), a solution of Br2 (0.69 g, 4.3 mmol) in CHCl3 (3 mL) was added under argon atmosphere. Acetonitrile (4 mL) was added and the mixture was stirred at room temperature for 2 days. The residue was concentrated, dissolved in CHCl3 and washed with 1 N NaOH. A precipitate was formed, which was filtered and dissolved with MeOH. The solution was concentrated and washed with 1 N NaOH. It was extracted with EtOAc, dried over Na2SO4 and concentrated. This was treated with diethyl ether, the solvent was decanted and the product obtained was dried to afford 1.16 g of the title compound (yield: 97%).

1. concentrationThe residue was concentrated
2. dissolutiondissolved in CHCl3
3. washwashed with 1 N NaOH
4. customA precipitate was formed
5. filtrationwhich was filtered
6. dissolutiondissolved with MeOH
7. concentrationThe solution was concentrated
8. washwashed with 1 N NaOH
9. extractionIt was extracted with EtOAc
10. dry with materialdried over Na2SO4
11. concentrationconcentrated
12. additionThis was treated with diethyl ether
13. customthe solvent was decanted
14. customthe product obtained
15. customwas dried