反应详情

温度

100 °C

A 250-mL single-neck round-bottomed flask equipped with a magnetic stirrer and reflux condenser was charged with 1,4-dioxane (60 mL), tert-butyl 4-(6-aminopyridin-3-yl)piperazine-1-carboxylate (1.5 g, 5.39 mmol), 8-bromo-6-chloroimidazo[1,2-a]pyridine 101a (3.7 g, 16.18 mmol), and cesium carbonate (3.52 g, 10.79 mmol). XantPhos (312 mg, 0.539 mmol) and Pd2(dba)3 (494 mg, 0.539 mmol) were added, and the reaction mixture was heated at 100° C. for 5 h under nitrogen. After this time the reaction was cooled to room temperature. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was purified on flash column eluting with 100:1 CH2Cl2/MeOH to afford 102a (1.8 g, 78%). MS: [M+H]+ 429.

1. customA 250-mL single-neck round-bottomed flask equipped with a magnetic stirrer
2. temperaturereflux condenser
3. temperatureAfter this time the reaction was cooled to room temperature
4. filtrationThe mixture was filtered
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified on flash column
7. washeluting with 100:1 CH2Cl2/MeOH