反应详情

Pyrrolidine (8.35 ml, 7.11 g, 0.1 mol) was added to a suspension of 2'-hydroxy-5'-methoxyacetophenone (16.62 g, 0.1 mol) in methanol (100 ml). The mixture was stirred for 10 minutes, then 1-benzoyl-4-piperidone (20.32 g, 0.1 mol) was added and the mixture was heated under reflux for 7 hr. The mixture was cooled and the solvent was evaporated under reduced pressure. Water (400 ml) was added and the mixture was extracted with ethyl acetate (3×400 ml). The combined organic fractions were evaporated under reduced pressure and the residue was recrystallized from methanol to give the ketone as a pale yellow solid (29.54 g, 84%).

1. temperaturethe mixture was heated
2. temperatureunder reflux for 7 hr
3. temperatureThe mixture was cooled
4. customthe solvent was evaporated under reduced pressure
5. additionWater (400 ml) was added
6. extractionthe mixture was extracted with ethyl acetate (3×400 ml)
7. customThe combined organic fractions were evaporated under reduced pressure
8. customthe residue was recrystallized from methanol