反应详情

温度

100 °C

A mixture of 8-bromo-2-chloro-[1,2,4]triazolo[1,5-a]pyridine (0.23 g, 0.99 mmol), 2-methoxy-5-trifluoromethyl-phenylamine (0.226 g, 1.19 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.185 g, 0.2 mmol), dicyclohexyl-(2′-4′-6′-triisopropyl-biphenyl-2-yl)-phosphane (0.19 g, 0.4 mmol), and sodium tert-butoxide (0.29 g, 3.0 mmol) in toluene (10 mL) was degassed with nitrogen for 3 minutes, then heated at 100° C. for 2 hours under argon. The reaction was cooled to room temperature, diluted with dichloromethane, filtered through diatomaceous earth, and concentrated. The residue was diluted with dichloromethane, washed with 10% sodium bicarbonate solution, brine, dried over sodium sulfate and concentrated. The crude product was triturated with ether and dichloromethane to give (2-chloro-[1,2,4]triazolo[1,5-a]pyridine-8-yl)-(2-methoxy-5-trifluoromethyl-phenyl)-amine (0.23 g, 68%). MP=144-146° C. MS=343 (MH)+.

1. customwas degassed with nitrogen for 3 minutes
2. temperatureThe reaction was cooled to room temperature
3. additiondiluted with dichloromethane
4. filtrationfiltered through diatomaceous earth
5. concentrationconcentrated
6. additionThe residue was diluted with dichloromethane
7. washwashed with 10% sodium bicarbonate solution, brine
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated
10. customThe crude product was triturated with ether and dichloromethane