反应详情

温度

80 °C

To a mixture of 4-hydroxybenzaldehyde (6.1 g), potassium carbonate (13.8 g), sodium iodide (0.75 g) and dimethylformamide (110 ml) was added N-(ethoxycarbonylmethyl)-2-chloroacetamide (8.9 g), and the mixture was stirred at 80° C. for 30 minutes. The reaction mixture was poured into 3% hydrochloric acid and extracted with ethyl acetate. The ethyl acetate layer was washed successively with water and a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. After evaporation of the solvent under reduced pressure, the residue was chromatographed on silica gel column (eluent; ethyl acetate), the desired fractions were collected and recrystallized from ethyl acetate/hexane to give N-(ethoxycarbonylmethyl)-2-(4-formylphenoxy)acetamide (4.09 g).

1. extractionextracted with ethyl acetate
2. washThe ethyl acetate layer was washed successively with water
3. dry with materiala saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate
4. customAfter evaporation of the solvent under reduced pressure
5. customthe residue was chromatographed on silica gel column (eluent; ethyl acetate)
6. customthe desired fractions were collected
7. customrecrystallized from ethyl acetate/hexane