反应详情

A mixture of 5 g (0.0197 mol) of the product obtained in Stage 2, 4 g (0.0216 mol) of 3-(4-fluorobenzoylmethyl)pyrrolidine, 0.1 g of sodium iodide and 3 g of potassium carbonate in 100 ml of diethyl ketone is brought to reflux for 24 hours. The inorganic salts are then filtered off, the solvent is evaporated under vacuum, the residue is taken up in 100 ml of dichloromethane and this organic phase is washed with 100 ml of water. After drying over magnesium sulfate and evaporation of the solvent, the residue is purified by chromatography on a silica column, Merck 70-230 mesh, using a dichloromethane/methanol/aqueous ammonia (97/3/0.3) mix-ture as eluent.

1. temperatureto reflux for 24 hours
2. filtrationThe inorganic salts are then filtered off
3. customthe solvent is evaporated under vacuum
4. washthis organic phase is washed with 100 ml of water
5. dry with materialAfter drying over magnesium sulfate and evaporation of the solvent
6. customthe residue is purified by chromatography on a silica column, Merck 70-230 mesh
7. additionmix-ture as eluent