反应详情

温度

90 °C

A mixture of ethyl acetoacetate [VI-1] (109.3 g), n-heptane (100 g) and 1-bromo-5-chloropentane [V-1] (185.5 g) is heated to 90° C. Thereto is added anhydrous potassium carbonate (193.5 g) in portions, and the mixture is stirred with heating at 100° C. for 14 hours. The mixture is filtered with suction, and the residue is washed with n-heptane. The n-heptane layers (i.e. the above filtrate and washing liquid) are combined to give a solution (347 g) of crude ethyl 7-chloro-2-(1-oxoethyl)heptanoate [II-1] in n-heptane (content of the heptanoate; 44.3 %).

1. temperaturewith heating at 100° C. for 14 hours
2. filtrationThe mixture is filtered with suction
3. washthe residue is washed with n-heptane
4. washThe n-heptane layers (i.e. the above filtrate and washing liquid)