反应详情

温度

50 °C

4-(1-Benzyloxymethyl-1H-pyrazolo[3,4-b]pyridin-4-yloxy)aniline (140 mg, 0.40 mmol) was dissolved in methanol (5 mL) and 5 N hydrochloric acid (0.2 mL), and palladium carbon (10%, 10 mg) was added thereto. The resulting mixture was stirred at 50° C. for 4 hours under a hydrogen atmosphere. The catalyst was removed by filtration, and the methanol solution was concentrated. The residue was neutralized with a 5 N sodium hydroxide aqueous solution (0.2 mL) and partitioned between saturated brine (3 mL) and ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then concentrated. The residue was purified by amino-silica gel (Fuji Silysia, 5 g, ethyl acetate) to give 4-(1H-pyrazolo[3,4-b]pyridin-4-yloxy)aniline (23 mg, yield: 25%).

1. customThe catalyst was removed by filtration
2. concentrationthe methanol solution was concentrated
3. custompartitioned between saturated brine (3 mL) and ethyl acetate
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customThe residue was purified by amino-silica gel (Fuji Silysia, 5 g, ethyl acetate)