反应详情

A solution of sodium ethoxide in ethanol, prepared by dissolving 23.69 g (1.03 moles) of sodium in 800 ml of absolute alcohol, was treated slowly with ethyl acetoacetate. To this solution was added, in one portion, 308 g (1.04 moles) of N-(5-bromopentyl)phthalimide and the resulting mixture was refluxed for two hours and stirred overnight at 25°. The ethanol was stripped, 1500 ml of water was added to the residue, and the resulting mixture was extracted with 3×400 ml of ether. The ether layers were combined, dried over anhydrous sodium sulfate, filtered and stripped to give 350 g of light brown oil. This material was used in the next step without purification.

1. temperaturethe resulting mixture was refluxed for two hours
2. extractionthe resulting mixture was extracted with 3×400 ml of ether
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered