反应详情

温度

110 °C

A mixture of 1-ethyl-4-chloro-6-bromo-1H-pyrazolo[3,4-b]quinoline (6.5 g, 0.021 mol), cyclohexanemethylamine (5.46 g, 0.042 mol) and DMSO (20 ml) was heated at 110° C. overnight. The reaction mixture was cooled, poured into water and basified with NH4OH. The mixture was extracted with CH2Cl2 (2×100 ml) and the combined CH2Cl2 extracts were washed with brine, then evaporated to about 20 ml. The solution was purified by column chromatography on silica gel eluting with ethyl acetate to afford 8.0 g (98.8%) of 1-ethyl-6-bromo-N-(cyclohexylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine, m.p. 158°-160° C.

1. temperatureThe reaction mixture was cooled
2. extractionThe mixture was extracted with CH2Cl2 (2×100 ml)
3. washthe combined CH2Cl2 extracts were washed with brine
4. customevaporated to about 20 ml
5. customThe solution was purified by column chromatography on silica gel eluting with ethyl acetate