反应详情

温度

150 °C

A mixture of 4-((4-fluorobenzyl)oxy)pyridin-2(1H)-one (5 g), 6-bromo-2-ethyl-1-methyl-1H-benzimidazole (6.54 g), potassium carbonate (9.46 g), N,N′-dimethylethylenediamine (2.91 ml), copper iodide (1.3 g) and DMSO (100 ml) was stirred at 150° C. for 4 h. After cooling, the mixture was poured into 28% NH3 solution at 0° C. The precipitate was collected by filtration and dissolved in EtOAc/THF. The resulting solution was washed with brine, dried over MgSO4 and concentrated in vacuo. The residue was treated with activated carbon in MeOH, and recrystallized from MeOH/water to give the title compound (3.44 g) as a white solid.

1. temperatureAfter cooling
2. filtrationThe precipitate was collected by filtration
3. dissolutiondissolved in EtOAc/THF
4. washThe resulting solution was washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. additionThe residue was treated with activated carbon in MeOH
8. customrecrystallized from MeOH/water