反应详情

温度

120 °C

In 3 ml of N,N-dimethylformamide are suspended 0.28 g of methyl 2-[5-(2-hydroxy-4-isobutoxybenzoyl)-2-isobutoxyphenyl]acetate, 0.32 g of potassium carbonate and 0.23 ml of isopentyl iodide. The suspension is stirred at 120° C. for 2 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 thus obtained is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography (eluent; hexane:ethyl acetate=5:1) to obtain 0.17 g of methyl 2-[5-(4-isobutoxy-2-isopentyloxybenzoyl)-2-isobutoxyphenyl]-acetate as a colorless oily product.

1. customthe organic layer is separated
2. customThe organic layer thus obtained
3. washis 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=5:1)