反应详情

温度

85 °C

In 9 ml of N,N-dimethylformamide is dissolved 0.86 g of (2,4-diisobutoxyphenyl)(3-hydroxy-4-isobutoxyphenyl)methanone, to which is added 0.12 g of 60% sodium hydride. After elevating the temperature to 80° C., 0.52 ml of ethyl 2-bromoacetate is added, and the mixture thus obtained is stirred at 80-90° C. for 30 minutes. The reaction mixture is cooled to ambient temperature and 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 1.00 g of ethyl 2-[5-(2,4-diisobutoxybenzoyl)-2-isobutoxyphenoxy]acetate as a light yellow oily product.

1. customto 80° C.
2. customthe mixture thus obtained
3. temperatureThe reaction mixture is cooled to ambient temperature
4. customthe organic layer is separated
5. customThe organic layer thus obtained
6. washis washed with water and saturated aqueous solution of sodium chloride successively
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationthe solvent is distilled off under reduced pressure
9. customThe residue thus obtained
10. customis purified by silica gel column chromatography (eluent; hexane:ethyl acetate=5:1)