反应详情

温度

110 °C

In 50 ml of N,N-dimethylformamide are suspended 5.0 g of 3,5-dihydroxybenzoic acid, 29.8 g of potassium carbonate and 11 ml of isobutyl iodide. The mixture thus obtained is stirred at 110° C. for 7 hours. The reaction mixture is added to a mixture of ethyl acetate and water, pH is adjusted to 2 with 6 mol/L hydrochloric acid, and the organic layer is separated. The organic layer is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and then the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography (eluent; hexane:ethyl acetate=10:1) to obtain 2.6 g of isobutyl 3,5-diisobutoxybenzoate as a light yellow oily product.

1. customThe mixture thus obtained
2. customthe organic layer is separated
3. washThe organic layer is washed with water and saturated aqueous solution of sodium chloride successively
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent is distilled off under reduced pressure
6. customThe residue thus obtained
7. customis purified by silica gel column chromatography (eluent; hexane:ethyl acetate=10:1)