反应详情

6-Fluoro-7-iodo-1H-pyrazolo[4,3-b]pyridin-3-amine (2.0 g, 7.19 mmol) was combined with DMF (15 mL) and cooled to 0° C. before tert-butyl nitrite (1.709 mL, 14.39 mmol) was added. The reaction mixture was then warmed to room temperature and heated at 85° C. for 4 hours. The reaction mixture was cooled to room temperature and HI solution (1.614 g, 7.19 mmol) in water (57%) was added and heated to 85° C. for another 8 hours. The mixture was cooled, concentrated, to give a residue which was purified by preparative HPLC using a Sunfire Prep 5 μm C18, 75×30 mm column eluting with a gradient of 25-45% acetonitrile (containing 10 mM NH4HCO3) in water (containing 10 mM NH4HCO3) to give the title compound. (221 mg, 0.840 mmol, 11.68% yield). MS [M+H] found 264.0.

1. additionwas added
2. temperatureheated at 85° C. for 4 hours
3. temperatureThe reaction mixture was cooled to room temperature
4. temperatureheated to 85° C. for another 8 hours
5. temperatureThe mixture was cooled
6. concentrationconcentrated
7. customto give a residue which
8. customwas purified by preparative HPLC
9. washeluting with a gradient of 25-45% acetonitrile (containing 10 mM NH4HCO3) in water (containing 10 mM NH4HCO3)