反应详情

温度

100 °C

Iron (2.41 g, 42.3 mmol) and ammonium chloride (2.58 g, 48.4 mmol) are added to a solution of 5-nitro-1-(tetrahydro-2H-pyran-4-yl)-1H-pyrazolo[3,4-b]pyridine (3 g, 12 mmol) in ethanol/THF/H2O (4:2:1, 35 mL). The mixture is heated at 100° C. for 2 h. The iron is removed by filtration through pad of Celite® and the filtrate was evaporated under reduced pressure. The residue is purified by flash column chromatography using a gradient of 70% ethyl acetate/petroleum ether to afford the title compound as an off-white solid (2.85 g, 93%).

1. customThe iron is removed by filtration through pad of Celite®
2. customthe filtrate was evaporated under reduced pressure
3. customThe residue is purified by flash column chromatography