反应详情

温度

150 °C

A mixture of 4-(benzyloxy)pyridin-2(1H)-one (1.60 g), 6-bromo-2-cyclopropyl-1-methyl-1H-benzimidazole (2 g), potassium carbonate (3.30 g), N,N′-dimethylethylenediamine (0.855 ml), copper iodide (1.52 g) and DMSO (40 ml) was stirred at 150° C. under Ar atmosphere for 1 h. The mixture was poured into 28% NH3 solution. The precipitate was collected by filtration and washed with water and EtOAc. The solid was dissolved in THF, put on through silica gel pad and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/MeOH). The resulting solid was dissolved in MeOH, and stirred with activated charcoal at room temperature for 10 min. The insoluble material was removed by filtration, and the filtrate was concentrated in vacuo to give the title compound (1.60 g) as an off-white solid.

1. filtrationThe precipitate was collected by filtration
2. washwashed with water and EtOAc
3. dissolutionThe solid was dissolved in THF
4. concentrationconcentrated in vacuo
5. customThe residue was purified by silica gel column chromatography (EtOAc/MeOH)
6. dissolutionThe resulting solid was dissolved in MeOH
7. stirringstirred with activated charcoal at room temperature for 10 min
8. customThe insoluble material was removed by filtration
9. concentrationthe filtrate was concentrated in vacuo