反应详情

To a solution of 93.10 g (0.47 mole) 1-(4-chlorophenyl)-1,3-butanedione in 500 ml acetone add 60.0 g (0.39 mole) 2-methylene-3-quinuclidinone. Stir the solution at reflux for about 24 hours. Follow the progress of the reaction by thin-layer chromatography on silica gel (EtOAc:MeOH, 9:1). At the completion of the reaction, chill the solution in an ice/water bath. Acidify dropwise with 35 ml concentrated hydrochloric acid to precipitate the product. Collect the precipitate by filtration to obtain the title compound as a mixture of diastereomers.

1. temperatureat reflux for about 24 hours
2. customthe progress of the reaction by thin-layer chromatography on silica gel (EtOAc:MeOH, 9:1)
3. customAt the completion of the reaction
4. temperaturechill the solution in an ice/water bath
5. customto precipitate the product
6. customCollect the precipitate
7. filtrationby filtration