反应详情

温度

70 °C

A 250 mL round-bottomed flask was charged with 1-(4-methoxybenzyl)-3-methyl-4-(5-nitropyrimidin-2-yloxy)-1H-pyrazolo[3,4-b]pyridine (0.420 g, 1.07 mmol), SnCl2 dihydrate (1.45 g, 6.42 mmol), and EtOH (100 mL). The reaction mixture was heated to 70° C. under nitrogen for 2 hours, then concentrated in vacuo. The residue was diluted with EtOAc, water, and brine. Aqueous saturated Na2CO3 was added until the pH was in the 9-10 range. The combined organic phases were dried (Na2SO4). The product was isolated by filtration and flash chromatography (EtOAc/MeOH 95:5) to afford 0.10 g (25%). LRMS M+1 (363.0) observed.

1. concentrationconcentrated in vacuo
2. additionThe residue was diluted with EtOAc, water, and brine
3. additionAqueous saturated Na2CO3 was added until the pH
4. dry with materialThe combined organic phases were dried (Na2SO4)
5. customThe product was isolated by filtration and flash chromatography (EtOAc/MeOH 95:5)
6. customto afford 0.10 g (25%)