反应详情

温度

90 °C

To a solution of compound 1e (600 mg, 1.92 mmol, as prepared in Step E) in 1,4-dioxane/H2O (4:1 v/v, 8 mL) was added compound 1f (560 mg, 2.44 mmol), PdCl2(dppf) (72.1 mg, 0.0960 mmol) and Cs2CO3 (847 mg, 4.99 mmol). The reaction mixture was stirred at 90° C. for 2 h under a nitrogen atmosphere. After cooling to rt, the reaction was quenched with H2O (20 mL). The resulting mixture was extracted with DCM (2×50 mL). The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure. The resulting residue was purified by flash column chromatography on silica gel with EtOAc/petroleum ether (1:2 v/v) to obtain compound 1g as a yellow solid (350 mg, 51% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C17H16N6O2: 337.1 (M+H). Found 337.2.

1. temperatureAfter cooling to rt
2. customthe reaction was quenched with H2O (20 mL)
3. extractionThe resulting mixture was extracted with DCM (2×50 mL)
4. dry with materialThe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue was purified by flash column chromatography on silica gel with EtOAc/petroleum ether (1:2 v/v)