反应详情

温度

70 °C

1-(4-Methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-4-ol (759 mg) was dissolved in phosphorus oxychloride (6 mL). The resulting mixture was stirred at 70° C. for 1 hour. The reaction solution was concentrated under reduced pressure. The residue was diluted with ethyl acetate and carefully washed with a sodium bicarbonate solution. The organic layer was dried (using sodium sulfate), and the drying agent was removed by filtration. The filtrate was concentrated under reduced pressure. The obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate=5/0 to 3/1) to give 4-chloro-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridine (568 mg, yield: 70%) as a colorless solid.

1. concentrationThe reaction solution was concentrated under reduced pressure
2. additionThe residue was diluted with ethyl acetate
3. washcarefully washed with a sodium bicarbonate solution
4. dry with materialThe organic layer was dried (using sodium sulfate)
5. customthe drying agent was removed by filtration
6. concentrationThe filtrate was concentrated under reduced pressure
7. customThe obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate=5/0 to 3/1)