反应详情

2′, 5′-Dihydroxyacetophenone (II-1) (15.22 g, 0.100 mol), benzyl bromide (17.96 g, 0.105 mol) and potassium carbonate (14.51 g, 0.105 mol) in acetone (200 ml) were refluxed for 16 h. After the solvent was removed under reduced pressure, water was added and the residue was extracted three times with ethyl acetate. The ethyl acetate layer was washed with water and brine, dried over magnesium sulfate, and the solvent removed under reduced pressure. The residue was purified by chromatography on silica gel (500 g) eluting with ethyl acetate/hexane=1:4 to give compound (II-2) as yellow crystals (20.96 g, 87%) accompanied by a small amount of di-benzyl derivative. The products were used without further purification. NMR(CDCl3): 2.57(3H, s), 5.04(2H, s), 6.92(1H, d, J=8.8), 7.14-7.31(2H, m), 7.34-7.45(5H, m)

1. customAfter the solvent was removed under reduced pressure, water
2. additionwas added
3. extractionthe residue was extracted three times with ethyl acetate
4. washThe ethyl acetate layer was washed with water and brine
5. dry with materialdried over magnesium sulfate
6. customthe solvent removed under reduced pressure
7. customThe residue was purified by chromatography on silica gel (500 g)
8. washeluting with ethyl acetate/hexane=1:4