反应详情

4 g of 4-(2,3-epoxypropoxy)-9-fluorenone are heated to 150° in an autoclave for 15 hours together with 4 g of 2,2,5,5-tetramethylpyrrolidine in 30 cc of dioxane. After cooling, the reaction mixture is concentrated by evaporation. The residue is taken up in ether and extracted with 2 N hydrochloric acid. The aqueous solution is made alkaline and thoroughly extracted with methylene chloride. The methylene chloride phase is concentrated by evaporation and the residue is crystallized from ethyl acetate/petroleum ether. The title compound has an M.P. of 137°-139°.

1. temperatureAfter cooling
2. concentrationthe reaction mixture is concentrated by evaporation
3. extractionextracted with 2 N hydrochloric acid
4. extractionthoroughly extracted with methylene chloride
5. concentrationThe methylene chloride phase is concentrated by evaporation
6. customthe residue is crystallized from ethyl acetate/petroleum ether