反应详情

温度

97.5 °C

Into 50 mL of glacial acetic acid, 3.7 g of 1-methoxy-5-phenoxynaphthalene prepared as above, followed by 20 mL of 40% aqueous hydrogen bromide was stirred. The mixture was heated at 95-100° C. for 16 hours. The solvent was removed under vacuum, and the residue was redissolved in ethyl acetate and washed three times with brine. The organic layer was dried over magnesium sulfate and filtered. After removing solvent, the residue was chromatographed over silica gel with a gradient elution of 0 to 30% ethyl acetate in hexane, providing 2.10 g (59%) of 1-hydroxy-5-phenoxynaphthalene.

1. customThe solvent was removed under vacuum
2. dissolutionthe residue was redissolved in ethyl acetate
3. washwashed three times with brine
4. dry with materialThe organic layer was dried over magnesium sulfate
5. filtrationfiltered
6. customAfter removing solvent
7. customthe residue was chromatographed over silica gel with a gradient elution of 0 to 30% ethyl acetate in hexane