反应详情

温度

70 °C

In a dry 25 mL round bottom flask, 7-(2-chloro-5-methoxy-phenyl)-5-methyl-benzo[1,2,4]triazin-3-ylamine (0.282 g, 0.94 mmol, 1 equiv), (4-bromo-phenyl)-(4-methyl-piperazin-1-yl)-methanone (0.399 g, 1.41 mmol, 1.5 equiv), cesium carbonate (0.919 g, 2.82 mmol, 3 equiv), 4,5-bis(diphenylphosphino)-9,9-dimethyl xanthene (0.109 g, 0.188 mmol, 0.2 equiv) and tris(dibenzylideneacetone)dipalladium (0.086 g, 0.094 mmol, 0.1 equiv) were combined. The reactants were flushed with argon, diluted with dioxane (12 mL) and outfitted with reflux condenser. The reaction was heated to reflux for 18 hours, then filtered hot and solvents were evaporated. The residue was diluted with toluene and water (approx. 2:1), and the mixture was heated to 70° C. and stirred for 20 min. The contents were then poured into 250 mL separatory funnel and shaken. The resulting precipitate was filtered off, washed with water and dried to yield a yellow powder (0.275 g, 58% yield). MS (ESI+): m/z=504.1, LC retention time: 1.75 min.

1. customThe reactants were flushed with argon
2. additiondiluted with dioxane (12 mL)
3. temperaturewith reflux condenser
4. temperatureThe reaction was heated
5. temperatureto reflux for 18 hours
6. filtrationfiltered hot
7. customsolvents were evaporated
8. additionThe residue was diluted with toluene and water (approx. 2:1)
9. additionThe contents were then poured into 250 mL separatory funnel
10. stirringshaken
11. filtrationThe resulting precipitate was filtered off
12. washwashed with water
13. customdried