反应详情

To a solution of 1-(triphenylmethyl)piperidin-4-one (3.66 g) in benzene (40 ml) was added pyrrolidine (0.97 ml), and the mixture was heated under reflux for 3.5 hours. To this mixture was added a solution of ethyl(5-formyl-1H-imidazol-1-yl)acetate (1.95 g) in benzene (10 ml) under cooling using an ice bath. Then, the whole was heated further under reflux for 8.5 hours. After cooling, the mixture was partitioned between water and ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The extract was concentrated under reduced pressure and the residue was purified by silica gel chromatography using hexane and ethyl acetate (1:3) as an eluent to afford the title compound (1.0 g, yield: 19%) as a yellow oil.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 3.5 hours
3. temperatureunder cooling
4. temperatureThen, the whole was heated further
5. temperatureunder reflux for 8.5 hours
6. temperatureAfter cooling
7. customthe mixture was partitioned between water and ethyl acetate
8. washThe organic layer was washed with a saturated aqueous sodium chloride solution
9. dry with materialdried over anhydrous magnesium sulfate
10. concentrationThe extract was concentrated under reduced pressure
11. customthe residue was purified by silica gel chromatography