反应详情

In 18 ml of methylene chloride is dissolved 1.8 g of 2-isobutoxy-4-(isobutoxycarbonyl)-benzoic acid. After adding 0.7 ml of oxalyl chloride and subsequently 20 μl of N,N-dimethylformamide at ambient temperature, the mixture thus obtained is stirred at ambient temperature for one hour. Then, 1.6 g of aluminum chloride and subsequently 1.8 g of ethyl 3-(2-isobutoxyphenyl)propanoate are added at 5-10° C., and the resulting mixture is stirred at ambient temperature for one hour. The reaction mixture is added to a mixture of chloroform and water 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 2.1 g of isobutyl 4-[3-(3-ethoxy-3-oxopropyl)-4-isobutoxybenzoyl]-3-isobutoxybenzoate as a colorless oily product.

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