反应详情

An oven dried 25 mL round bottom flask was charged with 7-bromo-5-methyl-benzo[1,2,4]triazin-3-ylamine (0.889 g, 3.72 mmol, 1 equiv), 3-(methylsulfonylamino) phenyl boronic acid (1.12 g, 5.21 mmol, 1.4 equiv), sodium carbonate (1.57 g, 14.9 mmol, 4 equiv) and tetrakis(triphenylphosphine)palladium(0) (0.43 g, 0.372 mmol, 0.1 equiv). The reactants were flushed with argon and diluted with ethylene glycol dimethyl ether (20 mL), ethanol (5 mL) and DI water (5 mL). The reaction vessel was outfitted with condenser and refluxed for 4 hours. The reaction was filtered hot and diluted with ethyl acetate. The Organic layer was isolated and concentrated to a dark residue. This was dissolved in DMF (6 mL) and slowly diluted with water so as to precipitate out the product. Solids were filtered off and dried to yield an orange solid (1 g, 82% yield).

1. customAn oven dried 25 mL round bottom flask
2. customThe reactants were flushed with argon
3. additiondiluted with ethylene glycol dimethyl ether (20 mL), ethanol (5 mL) and DI water (5 mL)
4. customThe reaction vessel was outfitted with condenser
5. temperaturerefluxed for 4 hours
6. filtrationThe reaction was filtered hot
7. additiondiluted with ethyl acetate
8. customThe Organic layer was isolated
9. concentrationconcentrated to a dark residue
10. dissolutionThis was dissolved in DMF (6 mL)
11. additionslowly diluted with water so as
12. customto precipitate out the product
13. filtrationSolids were filtered off
14. customdried