反应详情

温度

55 °C

To a solution of 1-(4-cyano-3-fluorobenzyl)-5-(acetoxymethyl)-imidazole hydrobromide (0.29 g, 1.06 mmol) in DMF (7.0 mL) was added 2-chlorophenol (0.132 mL, 1.27 mmol) and cesium carbonate (0.691 g, 2.12 mmol). The mixture was heated to 55° C. and stirred for 18 hr. The DMF was removed in vacuo and the residue was partitioned with EtOAc and saturated NaHCO3 solution. The EtOAc layer was washed with H2O, brine, and dried (MgSO4). Filtration and concentration to dryness gave the title compound after chromatography (SiO2, CH2Cl2:CH3OH: NH4OH/98:2:0.2) and conversion to the hydrochloride salt.

1. customThe DMF was removed in vacuo
2. customthe residue was partitioned with EtOAc and saturated NaHCO3 solution
3. washThe EtOAc layer was washed with H2O, brine
4. dry with materialdried (MgSO4)
5. filtrationFiltration and concentration to dryness