反应详情

温度

50 °C

A flask was charged with powdered potassium hydroxide (21.89 g, 390.2 mmol), benzoic acid (47.65 g, 390.2 mmol), and DMF (500 mL). The mixture was heated at 50° C. for 1 hour. 3-Chloropentane-2,4-dione (52.5 g, 390.2 mmol) was added and the reaction was stirred 50° C. overnight. The reaction was cooled to ambient temperature, diluted in water (1.5 L) and extracted with ether (3×500 mL). The combined organic layers were washed with water, saturated NH4Cl and brine. The organic layer was dried over sodium sulfate and concentrated in vacuo to afford 2,4-dioxopentan-3-yl benzoate (82.59 g, 96.12% yield) as yellow oil.

1. temperatureThe reaction was cooled to ambient temperature
2. extractionextracted with ether (3×500 mL)
3. washThe combined organic layers were washed with water, saturated NH4Cl and brine
4. dry with materialThe organic layer was dried over sodium sulfate
5. concentrationconcentrated in vacuo