反应详情

To 1-[1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]ethanone (3.14 g) was added trifluoroacetic acid (20 mL), and the mixture was heated to reflux for 2 days. The reaction solution was concentrated under reduced pressure. The resulting residue was diluted with ethyl acetate, and then sequentially washed with aqueous saturated sodium hydrogen carbonate solution and saturated saline, dried over magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=95/5→7/3) to give 1-(1H-pyrazolo[3,4-b]pyridin-3-yl)ethanone) [REx(103-1)] (1.73 g) as a pale yellow powder.

1. temperaturethe mixture was heated
2. temperatureto reflux for 2 days
3. concentrationThe reaction solution was concentrated under reduced pressure
4. additionThe resulting residue was diluted with ethyl acetate
5. washsequentially washed with aqueous saturated sodium hydrogen carbonate solution and saturated saline
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=95/5→7/3)