反应详情

温度

80 °C

To a solution of (trans-4-((6-bromo-3-(cyclopropanecarbonyl)quinolin-4-yl)amino)cyclohexyl)methyl methanesulfonate (362 mg, 0.75 mmol) and 3-hydroxypyrrolidine (262 mg, 3.0 mmol) in acetonitrile (15 mL) was added N,N-diisopropylethylamine (1.0 mL, 5.8 mmol) and the reaction mixture was heated at 80° C. for 16 h. The solution was cooled to room temperature, diluted satd. aq. NaHCO3 and extracted with ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate, concentrated and purified by column chromatography (silica, 0-20% methanol/dichloromethane) to afford the desired product (174 mg, 49%) as an off-white solid. ESI MS m/z 472 [C24H30BrN3O2+H]+

1. temperatureThe solution was cooled to room temperature
2. additiondiluted
3. extractionaq. NaHCO3 and extracted with ethyl acetate
4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
5. concentrationconcentrated
6. custompurified by column chromatography (silica, 0-20% methanol/dichloromethane)