反应详情

4-Bromomethyl-2-fluoro-benzonitrile, as described in Step D above, (3.44 g, 16.0 mmol) and imidazole (5.47 g, 80.3 mmol) were dissolved in DMF (40 mL) and stirred at ambient temperature for 2 h. The DMF was removed in vacuo and the residue was partitioned between EtOAc (300 mL) and aqueous saturated NaHCO3 solution. The organic layer was separated, washed with NaHCO3 solution, H2O, brine, and dried (MgSO4). Filtration and concentration to dryness gave the title compound after chromatography (silica gel, 1-2% CH3OH/CH2Cl2).

1. customThe DMF was removed in vacuo
2. customthe residue was partitioned between EtOAc (300 mL) and aqueous saturated NaHCO3 solution
3. customThe organic layer was separated
4. washwashed with NaHCO3 solution, H2O, brine
5. dry with materialdried (MgSO4)
6. filtrationFiltration and concentration to dryness