反应详情

To 100 ml of ethanol solution containing 14.0 g (26.8 mmol) of ethyl 2-[2-(3-cyclopropylmethoxy-4-difluoromethoxyphenyl)-2-oxoethyl]-4-(4-methoxybenzyloxy)-3-oxobutyrate obtained in Reference example 45-(b) was added 10.3 g (134 mmol) of ammonium acetate, the mixture was stirred at room temperature for 1 hour, and further stirred at 80° C. for 4 hours. After completion of the reaction, to the reaction mixture were added water and a saturated aqueous solution of sodium chloride, and the mixture was extracted with chloroform. The organic layer after separation was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The obtained residue was applied to silica gel column chromatography (Eluent; hexane:ethyl acetate=7:3 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 10.3 g of the title compound as a beige solid. (Yield: 77%)

1. stirringfurther stirred at 80° C. for 4 hours
2. customAfter completion of the reaction
3. extractiona saturated aqueous solution of sodium chloride, and the mixture was extracted with chloroform
4. customThe organic layer after separation
5. washwas washed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. additionthe fractions containing the desired compound
9. concentrationwere concentrated under reduced pressure