反应详情

温度

60 °C

1-(5-Ethenyl-6-methoxynaphthalen-2-yl)-1-(1-trityl-1H-imidazol-4-yl)-2-methyl-1-propanol (230 mg) was dissolved in a mixed solution of methanol and THF (3:1, 20 ml). To the solution was added pyridine hydrochloride (0.12 g), and the mixture was stirred at 60° C. for 3 h. The reaction mixture was concentrated to dryness, and to the residue were added ethyl acetate and 1N-hydrochloric acid (10 ml). The organic layer was extracted four times with 1N-hydrochloric acid. The aqueous layer was neutralized with an aqueous solution of sodium hydrogencarbonate and extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried and concentrated. The residue was purified by silica gel chromatography (eluent, dichloromethane-methanol=10:1) to give the titled compound (91 mg).

1. concentrationThe reaction mixture was concentrated to dryness
2. additionto the residue were added ethyl acetate and 1N-hydrochloric acid (10 ml)
3. extractionThe organic layer was extracted four times with 1N-hydrochloric acid
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with saturated sodium chloride solution
6. customdried
7. concentrationconcentrated
8. customThe residue was purified by silica gel chromatography (eluent, dichloromethane-methanol=10:1)