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 (40 mL), 5-methylisoxazol-3-amine (559 mg, 5.7 mmol), 4-bromo-6-chloro-2-methylpyridazin-3(2H)-one (1.89 g, 8.55 mmol), Pd2(dba)3 (521 mg, 0.57 mmol), XantPhos (329 mg, 0.57 mmol), and cesium carbonate (3.72 g, 11.4 mmol). After three cycles of vacuum/argon flush, the mixture was heated at 100° C. for 3 h. Then the mixture was cooled to 80° C. and filtered. The filtrate was cooled to room temperature. It was then filtered to afford 141a (600 mg, 44%) as a yellow solid. MS-ESI: [M+H]+ 241.0

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. temperatureThen the mixture was cooled to 80° C.
4. filtrationfiltered
5. temperatureThe filtrate was cooled to room temperature
6. filtrationIt was then filtered