反应详情

Sodium hydride (60% oil dispersion, 0.120 g) was added to DMF (15 ml), and to the mixture was slowly added 1-(6-hydroxynaphthalen-2-yl)-1-(1-trityl-1H-imidazol-4-yl)-2-methyl-1-propanol (1.397 g) under ice cooling, and the mixture was stirred for 30 min under ice cooling. To the mixture was added iodomethyl pivalate (0.83 g), and the mixture was stirred at room temperature for 6 h. To the mixture were added water and ethyl acetate, and the organic layer was washed with water and saturated solution of sodium chloride. The extract was dried and concentrated. The obtained residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=5:1→3:1). Recrystallization from hexane-ethyl acetate to give the titled compound (0.433 g) as a colorless solid.

1. stirringthe mixture was stirred at room temperature for 6 h
2. washthe organic layer was washed with water and saturated solution of sodium chloride
3. customThe extract was dried
4. concentrationconcentrated
5. customThe obtained residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=5:1→3:1)
6. customRecrystallization from hexane-ethyl acetate