反应详情

温度

120 °C

Palladium acetate (21 mg, 0.095 mmol) was added to a degassed solution of 3-methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline (155 mg, 0.76 mmol), ethyl 2-{2-chloro-6-[(2,2,2-trifluoro-ethoxy)methyl]pyrimidin-4-yl}acetate (180 mg, 0.63 mmol), Cs2CO3 (411 mg, 1.26 mmol), (2-biphenyl)dicyclohexylphosphine (33 mg, 0.95 mmol) in 1,4-dioxane (4 mL). The microwave tube was capped and the heterogeneous solution was immersed in a sonic bath for 2 min prior to heating it in a microwave reactor at 120° C. for 1.5 h. The reaction was cooled down to rt and concentrated in vacuo with diatomaceous earth. The resulting mixture was purified on silica gel eluting with 0% to 5% MeOH/DCM (1% ammonium hydroxide). The residue obtained was purified on a C18 reverse phase cartridge eluting with 0% to 40% MeOH/H2O (containing 0.05% TFA) to give the title compound as a gum, 110 mg (38%).

1. customThe microwave tube was capped
2. temperatureThe reaction was cooled down to rt
3. concentrationconcentrated in vacuo with diatomaceous earth
4. customThe resulting mixture was purified on silica gel eluting with 0% to 5% MeOH/DCM (1% ammonium hydroxide)
5. customThe residue obtained
6. customwas purified on a C18 reverse phase cartridge
7. washeluting with 0% to 40% MeOH/H2O (containing 0.05% TFA)