反应详情

温度

100 °C

7-(2-chloro-5-methoxy-phenyl)-5-methyl-benzo[1,2,4]triazin-3-ylamine (1.0 equiv., 0.75 mmol), 1-(4-bromo-benzenesulfonyl)-4-methyl-piperazine (1.5 equiv., 1.125 mmol), Xantphos (0.1 equiv., 0.074 mmol), palladium acetate (0.05 equiv., 0.0375 mmol), and potassium-tert-butoxide (2.0 equiv, 1.5 mmol) were dissolved in 20 mL of dioxane and bubbled with argon. The reaction was stirred in an oil bath at 100° C. for 18 h under an argon blanket. The reaction was cooled to room temperature and filtered to remove inorganics, concentrated under reduced pressure, then brought up in EtOAc and extracted using saturated NaHCO3 and brine. The organics were dried over Na2SO4 and concentrated under reduced pressure then precipitated using EtOAc/Hexanes (1:5 v/v) to afford brown solid (182.3 mg, 45% yield). MS (ES+): m/z=540 LC retention time: 2.67 min.

1. custombubbled with argon
2. temperatureThe reaction was cooled to room temperature
3. filtrationfiltered
4. customto remove inorganics
5. concentrationconcentrated under reduced pressure
6. extractionextracted
7. dry with materialThe organics were dried over Na2SO4
8. concentrationconcentrated under reduced pressure
9. customthen precipitated