反应详情

温度

115 °C

2-(3,4-Diaminophenyl)benzonitrile (9.6 mmoles, 2.0 g) was dissolved in 40 ml of pentafluoropropionic acid and heated at 115° C. for 20 hours. After cooling, the solvent was removed in vacuo. The residue was dissolved in ethyl acetate. The ethyl acetate solution was added slowly to saturated sodium bicarbonate. The intermediate was extracted with ethyl acetate, washed with brine, dried over sodium sulfate and concentrated. The residue was chromatographed over silica gel eluted with 25% ethyl acetate in hexane to yield 1.1 g of 5-(2-cyanophenyl)-2-pentafluoroethyl-1H-benzimidazole. (MS).

1. temperatureAfter cooling
2. customthe solvent was removed in vacuo
3. dissolutionThe residue was dissolved in ethyl acetate
4. additionThe ethyl acetate solution was added slowly to saturated sodium bicarbonate
5. extractionThe intermediate was extracted with ethyl acetate
6. washwashed with brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated
9. customThe residue was chromatographed over silica gel
10. washeluted with 25% ethyl acetate in hexane