反应详情

温度

50 °C

6-[1-Hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl]naphthalen-2-yloxymethyl 2,2-dimethylpropionate (0.381 g) was dissolved in acetic acid (15 ml). To the solution was added palladium carbon (0.200 g), and the mixture was stirred at 50° C. for 2 h under hydrogen atmosphere. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure. To the residue was added ethyl acetate, and the mixture was washed with saturated aqueous solution of sodium hydrogencarbonate and saturated sodium chloride solution. The organic layer was dried and concentrated. The obtained residue was purified by silica gel column chromatography (eluent, dichloromethane:methanol=30:1→20:1) to give the titled compound (0.107 g) as an amorphous product.

1. filtrationThe catalyst was filtered off
2. concentrationthe filtrate was concentrated under reduced pressure
3. additionTo the residue was added ethyl acetate
4. washthe mixture was washed with saturated aqueous solution of sodium hydrogencarbonate and saturated sodium chloride solution
5. customThe organic layer was dried
6. concentrationconcentrated
7. customThe obtained residue was purified by silica gel column chromatography (eluent, dichloromethane:methanol=30:1→20:1)