反应详情

To a stirred mixture of 2.14 g of β-dimethylaminopropiophenone hydrochloride and 1.92 g of ethyl benzoylacetate in 30 cc of ethanol was added in small portions 1.36 g of sodium ethoxide at room temperature. The resulting mixture was stirred at room temperature for 30 minutes and then heated under reflux for 1 hour. After cooling, the solvent was distilled off and water was added to the residue. The aqueous layer was acidified with 1N HCl, and extracted twice with chloroform. The combined organic layer was washed with a saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was distilled off and the crude product thus obtained was purified by a silica gel column chromatography (eluent: ethyl acetate/hexane=1/5) to obtain 2.45 g of compound G. Yield: 75.5%.

1. temperatureheated
2. temperatureunder reflux for 1 hour
3. temperatureAfter cooling
4. distillationthe solvent was distilled off
5. additionwater was added to the residue
6. extractionextracted twice with chloroform
7. washThe combined organic layer was washed with a saturated aqueous sodium chloride solution
8. dry with materialdried over magnesium sulfate
9. distillationThe solvent was distilled off
10. customthe crude product thus obtained
11. customwas purified by a silica gel column chromatography (eluent: ethyl acetate/hexane=1/5)