反应详情

温度

120 °C

In a microwave safe tube, 5-bromo-7-azaindole (81, 392 mg, 1.99 mmol), prepared from 7-azaindole following the published procedure (Marie-Claude, Viaud, Heterocycles, 1999, 50, 1065-1080), 3,4-dimethoxyphenyl boronic acid (905 mg, 4.97 mmol), and tetrakis(triphenylphosphine)palladium(0) (11 mg, 0.099 mol) were mixed in 1.0 M of potassium carbonate (6.0 mL) and tetrahydrofuran (9.5 mL, 0.12 mol). The resulting mixture was heated at 120° C. in a CEM Discover microwave unit for 10 minutes. Ethyl acetate and water were added, and the two layers were separated. The aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with brine and dried over anhydrous sodium sulfate. Concentration under reduced pressure afforded the crude material, which was purified by column chromatography (40-70% ethyl acetate:hexanes) to yield the desired product as a light yellow solid (82, 207 mg, 41%). MS(ESI) [M+H+]+=255.2.

1. customthe two layers were separated
2. extractionThe aqueous layer was extracted with ethyl acetate
3. washThe combined organic layers were washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationConcentration under reduced pressure
6. customafforded the crude material, which
7. customwas purified by column chromatography (40-70% ethyl acetate:hexanes)