反应详情

温度

100 °C

A 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and a reflux condenser was charged with 1,4-dioxane (25 mL), 155b (640 mg, 3.3 mmol), 4-bromo-6-chloro-2-methylpyridazin-3(2H)-one (1.1 g, 4.95 mmol), Pd2(dba)3 (302 mg, 0.33 mmol), XantPhos (381 mg, 0.66 mmol), and cesium carbonate (2.15 g, 6.6 mmol). After three cycles of vacuum/argon flush, the mixture was heated at 100° C. for 3 h. After this time the reaction was cooled to room temperature. It was then filtered and the filtrate was evaporated under reduced pressure. The residue was washed with ethyl acetate to afford 155c (754 mg, 68%) as a yellow solid. MS-ESI: [M+H]+ 337.3

1. customA 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and a reflux condenser
2. customAfter three cycles of vacuum/argon flush
3. temperatureAfter this time the reaction was cooled to room temperature
4. filtrationIt was then filtered
5. customthe filtrate was evaporated under reduced pressure
6. washThe residue was washed with ethyl acetate