反应详情

温度

80 °C

4-(4-hydroxyphenyl)butanoic acid methyl ester (2) (2.6 g) from the previous step was dissolved in N,N′-dimethylformamide (30 mL), 1,2-dibromoethane (12.6 g) and potassium carbonate (3.7 g) were added, and stirred at 80° C. for two days. The reaction solution was poured into water, and extracted with ethyl acetate (100 mL). The organic layer was washed with water (50 mL) and saturated sodium chloride solution (50 mL). After drying on anhydrous sodium sulfate, filtration and vacuum concentration, the residue was purified by silica gel flash column chromatography (developing solvent: n-hexane:ethyl acetate=8:1) to give the above-identified compound (676 mg, yield 17%).

1. extractionextracted with ethyl acetate (100 mL)
2. washThe organic layer was washed with water (50 mL) and saturated sodium chloride solution (50 mL)
3. dry with materialAfter drying on anhydrous sodium sulfate, filtration and vacuum concentration
4. customthe residue was purified by silica gel flash column chromatography (developing solvent: n-hexane:ethyl acetate=8:1)