反应详情

To a solution of ethyl 3-oxopentanoate (7.21 mL; 50 mmol) in dry DMF (25 mL) under nitrogen atmosphere was added potassium carbonate (7.6 g; 55 mmol), which has been dried at 120° C. for 12 h before using. After stirring for 15 min at room temperature, ethyl 2-bromovalerate (8.53 mL; 50 mmol) was slowly added under nitrogen and the mixture was vigorously stirred at room temperature for 24 h. The reaction mixture was poured in water (240 mL) and neutralized by adding a solution of hydrochloric acid 6N. The product was extracted with diethyl ether (2×240 mL) and the combined organic layers were dried over magnesium sulphate, filtered and concentrated under reduced pressure. Purification by distillation under reduced pressure furnished 7.9 g (58%) of the title compound as a colorless liquid (bp. 130-135° C., 4 mbar, temperature of the oil bath 150° C.).

1. customhas been dried at 120° C. for 12 h
2. stirringthe mixture was vigorously stirred at room temperature for 24 h
3. extractionThe product was extracted with diethyl ether (2×240 mL)
4. dry with materialthe combined organic layers were dried over magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customPurification
8. distillationby distillation under reduced pressure