反应详情

温度

125 °C

To a N,N-dimethylformamide (200 mL) solution of 4-benzyloxy-2-hydroxybenzaldehyde (18.6 g, 81.4 mmol) were added ethyl bromoacetate (9.94 mL, 89.6 mmol) and potassium carbonate (22.6 g, 163 mmol) at room temperature, which was stirred at 125° C. for 3 hours. To the reaction mixture was added water at room temperature followed by extraction with ethyl acetate. After washing the organic layer with water and sat. NaCl, the organic layer was dried over anhydrous magnesium sulfate and filtered followed by concentrating the filtrate under a reduced pressure. The residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=7:3) to obtain the title compound (18.4 g, 76%) as a white solid.

1. extractionfollowed by extraction with ethyl acetate
2. washAfter washing the organic layer with water and sat. NaCl
3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationby concentrating the filtrate under a reduced pressure
6. customThe residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=7:3)