反应详情

Benzyl 4-(4-iodobutyl)phenyl ether (14.29 g), 2-(2-hydroxyethyl)imidazole (13.1 g) and potassium carbonate (5.39 g) were stirred in DMF (390 ml) at 60° C. for 16 hours. After cooling, the insoluble matter was filtered off; the filtrate was concentrated under reduced pressure. The residue was dissolved in ethyl acetate and washed with water and saturated brine. Under reduced pressure, the solvent was distilled off; the residue was purified by column chromatography (eluent:ethyl acetate:methanol=19:1 to 9:1). The eluate was recrystallized from ethyl acetate-methanol to give the titled compound (10.99 g) as colorless crystals.

1. temperatureAfter cooling
2. filtrationthe insoluble matter was filtered off
3. concentrationthe filtrate was concentrated under reduced pressure
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed with water and saturated brine
6. distillationUnder reduced pressure, the solvent was distilled off
7. customthe residue was purified by column chromatography (eluent:ethyl acetate:methanol=19:1 to 9:1)
8. customThe eluate was recrystallized from ethyl acetate-methanol