反应详情

温度

60 °C

A mixture of tert-butyl 4-(5-cyclopropyl-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate (1.44 g, 4.2 mmol) and powdered potassium hydroxide (692 mg, 10.5 mmol) in DMF (20 mL) was treated with iodine (2.13 g, 8.39 mmol), and the mixture was heated at 60° C. for 5 hours. The mixture was cooled to room temperature, diluted with EtOAc (200 mL) and successively washed with a saturated Na2S2O3 solution (2×20 mL) and water (2×50 mL). The organic layer was separated, dried (MgSO4), filtered, and concentrated in vacuo to provide the crude tert-butyl 4-(5-cyclopropyl-3-iodo-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate (2 g, 102% yield) as a solid. LCMS (APCI+) m/z 470.1 (M+H)+.

1. temperatureThe mixture was cooled to room temperature
2. washsuccessively washed with a saturated Na2S2O3 solution (2×20 mL) and water (2×50 mL)
3. customThe organic layer was separated
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo