反应详情

A mixture of ethyl acetoacetate [VI-1] (260.2 g, 2.0 mol), methyl isobutyl ketone 300 9) and 1-bromo-5-chloropentane [V-1] (311.0 g, 1.68 mol) is heated to 80°-90° C. Thereto is added anhydrous potassium carbonate (300 g), and the mixture is reacted at 80°-90° C. for 12 hours. To the reaction mixture is further added potassium carbonate (341.4 g), and the mixture is reacted for additional 6 hours. After completion of the reaction, the mixture is filtered, and the methyl isobutyl ketone layer is washed with water and concentrated under reduced pressure. The residue (398.6 g) contains ethyl 7-chloro-2-(1-oxoethyl)-heptanoate (content; 70.8 %, yield; 72.6 %), which is purified by column chromatography to give pure ethyl 7-chloro-2-(1-oxoethyl)heptanoate [II-1].

1. temperatureis heated to 80°-90° C
2. customthe mixture is reacted at 80°-90° C. for 12 hours
3. customthe mixture is reacted for additional 6 hours
4. customAfter completion of the reaction
5. filtrationthe mixture is filtered
6. washthe methyl isobutyl ketone layer is washed with water
7. concentrationconcentrated under reduced pressure