反应详情

A mixture containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)pyrrolidine (0.5 g--see Preparation 8), 3,4-dimethylphenethyl bromide (0.4 g--see Preparation 18), anhydrous potassium carbonate (0.5 g) and acetonitrile (10 ml) was heated under reflux for 2 hours. On cooling to room temperature, water (80 ml) was added and the mixture was extracted with dichloromethane (3×70 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a yellow oil which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 4%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as an oil, yield, 0.22 g.

1. temperaturewas heated
2. temperatureunder reflux for 2 hours
3. extractionthe mixture was extracted with dichloromethane (3×70 ml)
4. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto give a yellow oil which
7. customwas purified by column chromatography on silica eluting with dichloromethane
8. additioncontaining methanol (0% up to 4%)
9. concentrationconcentrated in vacuo