反应详情

温度

0 °C

5-Aminonaphthalen-2-ol (356 mg, 2.24 mmol) was dissolved in DMF (2.5 mL) then cooled to 0° C. Sodium hydride (94 mg) was added slowly and the stirring was continued for 15 min at 0° C. 4-Iodo-1H-pyrazolo[3,4-b]pyridine (274 mg, 1.12 mmol) was then added slowly and the reaction was heated at 100° C. for 16 h, followed by 4.5 h at 120° C. The mixture was partitioned between water and EtOAc then washed with water, 1N aqueous NaOH, and brine. The organic layer was dried over sodium sulfate and concentrated in vacuo to give 6-(1H-pyrazolo[3,4-b]pyridin-4-yloxy)naphthalen-1-amine as a brown solid MS (ESI, pos. ion) m/z: 277.1 (M+1).

1. temperaturethe reaction was heated at 100° C. for 16 h
2. waitfollowed by 4.5 h at 120° C
3. customThe mixture was partitioned between water and EtOAc
4. washthen washed with water, 1N aqueous NaOH, and brine
5. dry with materialThe organic layer was dried over sodium sulfate
6. concentrationconcentrated in vacuo