反应详情

温度

50 °C

To a solution of 2-bromo-5-cyano-benzoic acid (200 mg, 0.885 mmol) in DMF (3 ml) was added dropwise 1,1′-Carbonyldiimidazole (148 mg, 0.885 mmol). When the CO2 evolution ceased, the mixture was heated to 50° C. for 15 minutes. The mixture was cooled to room temperature. 1-(3-Fluoro-4-piperazin-1-yl-phenyl)-ethanone (198 mg, 0.885 mmol) was added portionwise. The mixture was stirred at room temperature for 1 hour. The solvent was removed in vacuo. The residue was dissolved in ethyl acetate. The solution was washed twice with water, dried over Na2SO4, filtered and the solvent was removed in vacuo. The crude oil was purified on SiO2 (Heptane/AcOEt 0%-30% (10 minutes)) to provide 3-[4-(4-acetyl-2-fluoro-phenyl)-piperazine-1-carbonyl]-4-bromo benzonitrile (185 mg, 49%) as white solid (M+ 430.3).

1. temperatureThe mixture was cooled to room temperature
2. customThe solvent was removed in vacuo
3. dissolutionThe residue was dissolved in ethyl acetate
4. washThe solution was washed twice with water
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customthe solvent was removed in vacuo
8. customThe crude oil was purified on SiO2 (Heptane/AcOEt 0%-30% (10 minutes))