反应详情

温度

170 °C

A mixture of 6,7-dichloro-2,3-dimethoxy-5-(2-phenylethynyl)quinoxaline (2.0 g, 5.57 mmol) and trimethylsilyl azide (20 mL) was heated at 170° C. in a sealed vessel for 18 hours. After cooling, water (20 mL) was added followed by saturated aqueous sodium hydrogen carbonate solution (50 mL) and the mixture extracted with ethyl acetate (3×50 mL). The combined organic extracts were dried (MgSO4) and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel, by gradient elution using dichloromethane:methanol (1:0 changing to 98:2, by volume) to afford the title compound (1.3 g, 58%) as a brown foam.

1. temperatureAfter cooling
2. extractionthe mixture extracted with ethyl acetate (3×50 mL)
3. dry with materialThe combined organic extracts were dried (MgSO4)
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by flash chromatography on silica gel, by gradient elution