反应详情

A mixture of 1-ethyl-4-chloro-1H-pyrazolo[3,4-b]quinoline (0.7 g, 3 mmol), 4-[2-(4-morpholinyl)ethoxy]phenylmethylamine (0.75 g, 3.2 mmol) and DMSO (3 mL) was heated on a steam bath for 8 hours. Additional 1-ethyl-4-chloro-1H-pyrazolo[3,4-b]quinoline (0.7 g, 3 mmol) was then added and the reaction mixture was heated on a steam bath for another 4 hours. The reaction mixture was cooled to room temperature and then was poured into water. The mixture was extracted with CH2Cl2 (3×100 mL) and then CH2Cl2 layers were combined, dried over MgSO4 and evaporated to dryness. The residue was purified by column chromatography on silica gel eluting with CH2Cl2 /methanol (95/5), followed by recrystallization from ethyl acetate, to afford 1.0 g of 1-ethyl-N-[4-[2-(4-morpholinyl)ethoxy]phenylmethyl]-1H-pyrazolo[3,4-b]quinolin-4amine, as a yellow solid, m.p. 170°-172° C.

1. temperaturewas heated on a steam bath for 8 hours
2. temperaturethe reaction mixture was heated on a steam bath for another 4 hours
3. extractionThe mixture was extracted with CH2Cl2 (3×100 mL)
4. dry with materialdried over MgSO4
5. customevaporated to dryness
6. customThe residue was purified by column chromatography on silica gel eluting with CH2Cl2 /methanol (95/5)
7. customfollowed by recrystallization from ethyl acetate