反应详情

A mixture containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)piperidine (0.3 g), 4-chlorophenethyl bromide (0.24 g), anhydrous potassium carbonate (0.3 g) and acetonitrile (15 ml) was heated under reflux for 7 hours. The mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml), the layers separated, and the aqueous layer extracted with dichloromethane (2×50 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a solid which was recrystallised from aqueous methanol to give the title compound, yield 0.24 g, m.p. 188°-190° C.

1. temperaturewas heated
2. temperatureunder reflux for 7 hours
3. customThe mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml)
4. customthe layers separated
5. extractionthe aqueous layer extracted with dichloromethane (2×50 ml)
6. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
7. concentrationconcentrated in vacuo
8. customto give a solid which
9. customwas recrystallised from aqueous methanol