反应详情

Methanesulfonic anhydride (0.160 g, 0.922 mmol) was added to a slurry of 4-[(4-amino-2-ethyl-2H-pyrazolo[3,4-c]quinolin-1-yl)methyl]piperidin-4-ol (0.300 g, 0.922 mmol) in chloroform (10 mL). After 16 hours, 2M aqueous sodium carbonate was added and the biphasic mixture was stirred for 30 minutes resulting in a white precipitate. The mixture was extracted with 10% methanol in dichloromethane. The solution was concentrated. The residue was purified via automated flash chromatography and recrystallized from acetonitrile to provide 0.165 g of 4-[(4-amino-2-ethyl-2H-pyrazolo[3,4-c]quinolin-1-yl)methyl]-1-(methylsulfonyl)piperidin-4-ol as a white solid, mp 268-270° C.

1. customresulting in a white precipitate
2. extractionThe mixture was extracted with 10% methanol in dichloromethane
3. concentrationThe solution was concentrated
4. customThe residue was purified via automated flash chromatography
5. customrecrystallized from acetonitrile