反应详情

温度

120 °C

N-[6-Bromo-7-methyl-8-(3-trifluoromethyl-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-yl]-acetamide (Int. 18, 1.07 g, 2.59 mmol), bis(triphenylphosphine)palladium (II) dichloride (91 mg, 0.13 mmol) and tributyl(1-ethoxyvinyl) tin were suspended in dry DMF (8 mL) and degassed with argon. The reaction mixture was heated at 120° C. for 20 min using microwave irradiation. 1 M HCl (10 mL) was added and the reaction mixture was stirred for 1 hr before being partitioned between EtOAc (100 mL) and water (100 mL). The organic layer was washed with saturated brine, then dried (Na2SO4) and concentrated in vacuo to give a yellow solid. The solid was triturated with EtOAc and the solid collected by filtration, washing with EtOAc, to give the title compound as a cream solid (680 mg).

1. customdegassed with argon
2. custommicrowave irradiation
3. addition1 M HCl (10 mL) was added
4. custombefore being partitioned between EtOAc (100 mL) and water (100 mL)
5. washThe organic layer was washed with saturated brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo
8. customto give a yellow solid
9. customThe solid was triturated with EtOAc
10. filtrationthe solid collected by filtration
11. washwashing with EtOAc