反应详情

A mixture containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)pyrrolidine (0.5 g--see Preparation 8), 3-methylphenethylbromide (0.36 g--see J. Ind. Chem. Sac., 40, 327, (1963)) , anhydrous potassium carbonate (0.5 g) and acetonitrile (10 ml) was heated under reflux for 4 hours. On cooling to room temperature, water (60 ml) was added and the mixture was extracted with dichloromethane (3×50 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give an oil which was purified by column chromatography on silica eluting with dichloromethane containing methanol (2% up to 4%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as an oil, yield, 0.17 g.

1. temperaturewas heated
2. temperatureunder reflux for 4 hours
3. extractionthe mixture was extracted with dichloromethane (3×50 ml)
4. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto give an oil which
7. customwas purified by column chromatography on silica eluting with dichloromethane
8. additioncontaining methanol (2% up to 4%)
9. concentrationconcentrated in vacuo