反应详情

A solution of 21.6 g. of ethyl acetoacetate and 10 ml. of 1,2-dimethoxyethane is added to a suspension of 4.0 g. of sodium hydride in 1,2-dimethoxyethane under argon. A solution of 17.3 g. of 4-[15-(trifluoromethyl)pentadecylamino]benzoyl chloride hydrochloride in 1,2-dimethoxyethane is then added. The reaction mixture is refluxed for 5 hours, cooled, poured on ice and extracted with ether. The ether solution is washed with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated to dryness. Recrystallization from ether affords the product as a white solid.

1. temperatureThe reaction mixture is refluxed for 5 hours
2. temperaturecooled
3. additionpoured on ice
4. extractionextracted with ether
5. washThe ether solution is washed with water and saturated sodium chloride solution
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated to dryness
8. customRecrystallization from ether