反应详情

To 2.09 g 6-(4-methoxymethoxy-phenyl)-3-methyl-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carboxylic acid ethyl ester in 140 ml ethanol was added 100 ml of 1M aqueous sodium hydroxide solution. After 3 h at r.t. the volatiles were removed in vacuo. The residue was taken up in water and the pH was adjusted to 4-5. The aqueous phase was extracted with ethyl acetate three times. The combined organic phases were dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography (silica, dichloromethane/MeOH gradient with addition of aqueous ammonia) to obtain 1.74 g (90%) of the title compound.

1. customAfter 3 h at r.t. the volatiles were removed in vacuo
2. extractionThe aqueous phase was extracted with ethyl acetate three times
3. dry with materialThe combined organic phases were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by flash chromatography (silica, dichloromethane/MeOH gradient with addition of aqueous ammonia)