反应详情

To a solution of 3-cyclohexyl-N-(6′-fluoro-3-nitro-2′-trifluoromethyl-biphenyl-4-yl)-acrylamide (135 mg, 0.309 mmol, prepared as in STEP B above) in EtOH (4 mL) and HOAc (2 mL) was added Fe powder (86.3 mg, 1.54 mmol). The resulting mixture was heated at reflux overnight. The resulting mixture was allowed to cool to room temperature and filtered. The filtrate was concentrated. The residue was dissolved in DCM with heating and sonication. The DCM layer was washed with 10 mL saturated aqueous NaHCO3, separated, dried over Na2SO4 and concentrated. The residue obtained was purified on silica (EtOAc/hexane, 0:100 to 100:0, v/v) to yield 2-(2-Cyclohexyl-vinyl)-5-(2-fluoro-6-trifluoromethyl-phenyl)-1H-benzimidazole.

1. temperatureThe resulting mixture was heated
2. temperatureat reflux overnight
3. filtrationfiltered
4. concentrationThe filtrate was concentrated
5. dissolutionThe residue was dissolved in DCM
6. temperaturewith heating
7. customsonication
8. washThe DCM layer was washed with 10 mL saturated aqueous NaHCO3
9. customseparated
10. dry with materialdried over Na2SO4
11. concentrationconcentrated
12. customThe residue obtained
13. customwas purified on silica (EtOAc/hexane, 0:100 to 100:0