反应详情

A mixture of 30.5 g of 3-(4-fluorophenacyl)pyrrolidine (Chem. Pharm. Bull., 1977, 25(8), p. 1911-1922), 19.4 g of 2-bromoethanol, 15.6 g of sodium carbonate and 400 ml of acetonitrile is heated to reflux for 6 hours. The mixture is concentrated, the residue is taken up in 150 ml of aqueous saline, the product is extracted 5 times with 150 ml of dichloromethane and this organic phase is dried over anhydrous sodium sulfate and concentrated. The oil obtained is purified by chromatography on 650 g of silica (70-230 mesh), using a mixture of dichloromethane, methanol and ammonia solution (96:4:0.4 V/V) as eluant. A colorless oil is obtained.

1. temperatureis heated
2. temperatureto reflux for 6 hours
3. concentrationThe mixture is concentrated
4. extractionthe product is extracted 5 times with 150 ml of dichloromethane
5. dry with materialthis organic phase is dried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe oil obtained
8. customis purified by chromatography on 650 g of silica (70-230 mesh)
9. additiona mixture of dichloromethane, methanol and ammonia solution (96:4:0.4 V/V) as eluant
10. customA colorless oil is obtained