反应详情

To a suspension of 3-iodo-1H-pyrazolo[3,4-c]pyridine (6.24 g, 22.9 mmol) and potassium carbonate (7.29 g, 52.7 mmol) in acetonitrile (50 mL) was added tert-butyl bromoacetate (4.06 mL, 27.5 mmol) dropwise at RT and the resulting mixture was heated to reflux for 2 h. The mixture was cooled to RT and filtered, the solid was washed with CH3CN and the filtrate was concentrated under vacuum. The residual oil was purified by flash column chromatography on silica gel (gradient EtOAc/c-hexane 1:4, then 1:2, then 1:1). MS (LC/MS): 360.0 [M+H]+; tR (HPLC conditions k): 2.93 min.

1. temperaturethe resulting mixture was heated
2. temperatureto reflux for 2 h
3. filtrationfiltered
4. washthe solid was washed with CH3CN
5. concentrationthe filtrate was concentrated under vacuum
6. customThe residual oil was purified by flash column chromatography on silica gel (gradient EtOAc/c-hexane 1:4
7. custom2.93 min.