反应详情

A mixture contaiing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)pyrrolidine (0.6 g--g see Preparation 13), anhydrous potassium carbonate (0.5 g) and acetonitrile (20 ml) was heated under reflux for 1.5 hours. On cooling to room temperature, water (60 ml) was added and the mixture extracted with dichloromethane (3×50 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 6%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a colourless foam, yield, 0.25 g.

1. temperatureunder reflux for 1.5 hours
2. extractionthe mixture extracted with dichloromethane (3×50 ml)
3. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
4. concentrationconcentrated in vacuo
5. customto give a gum which
6. customwas purified by column chromatography on silica eluting with dichloromethane
7. additioncontaining methanol (0% up to 6%)
8. concentrationconcentrated in vacuo