反应详情

To a stirred solution of ethyl 6-bromo-1-isopropyl-1H-pyrazolo[3,4-b]pyridine-4-carboxylate (2 g, 6.43 mmol) in acetic acid (6 mL) was added bromine (5.14 g, 32.15 mmol) at 0° C. Resulting reaction mass was stirred at room temperature for 3 h. Reaction was monitored by TLC. On completion, reaction was quenched with ice, NaHCO3 solution was added to it. Extraction was carried out using ethyl acetate; the combined organic layers were washed with water, brine and dried over anhydrous Na2SO4. Solvent was removed under reduced pressure and residue was purified by silica gel column chromatography to obtain the desired intermediate (1.2 g, 48%).

1. customResulting
2. customreaction mass
3. customReaction
4. customOn completion, reaction
5. customwas quenched with ice, NaHCO3 solution
6. additionwas added to it
7. extractionExtraction
8. washthe combined organic layers were washed with water, brine
9. dry with materialdried over anhydrous Na2SO4
10. customSolvent was removed under reduced pressure and residue
11. customwas purified by silica gel column chromatography