反应详情

A mixture containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)pyrrolidine (0.5 g--see Preparation 8), 4-fluorophenethyl bromide (0.36 g--see J.A.C.S., 63, 602 (1941)), anhydrous potassium carbonate (0.5 g) and acetonitrile (15 ml) was heated under reflux for 2 hours. On cooling to room temperature, water (70 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 a glass 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 a colourless glass, yield, 0.056 g.

1. temperaturewas heated
2. temperatureunder reflux for 2 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 a glass which
7. customwas purified by column chromatography on silica eluting with dichloromethane
8. additioncontaining methanol (2% up to 4%)
9. concentrationconcentrated in vacuo