反应详情

温度

120 °C

Zinc cyanide (4.05 g), tris(dibenzylideneacetone)dipalladium (527 mg) and 1,1′-bis(diphenylphosphino)ferrocene (638 mg) were added to a solution of 1-(4-bromo-5-fluoro-2-methoxyphenyl)-4-methyl-1H-imidazole (16.7 g) obtained in Example 18 in DMF (100 mL) at room temperature, and the reaction solution was stirred with heat in a nitrogen atmosphere at 120° C. for 7 hours. Further, zinc cyanide (4.05 g), tris(dibenzylideneacetone)dipalladium (527 mg) and 1,1′-bis(diphenylphosphino)ferrocene (638 mg) were added to the reaction solution, and the reaction solution was stirred with heat for 7 hours. After allowing the reaction solution to be cooled, concentrated aqueous ammonia and ethyl acetate were added to the reaction solution and the organic layer was partitioned. The resulting organic layer was washed with brine, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate to obtain 9.5 g of the title compound. Properties data of the compound are as follows.

1. stirringthe reaction solution was stirred
2. temperaturewith heat for 7 hours
3. temperatureto be cooled
4. customthe organic layer was partitioned
5. washThe resulting organic layer was washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was recrystallized from ethyl acetate