反应详情

Combine 1-(3,4,5-trimethoxy-benzoyl)-3-(3,4-dichloro-phenyl)-3-(2-methanesulfonyl-ethyl)-pyrrolidine (0.20 g, 0.38 mmol) and 4-[1-(4-fluoro-benzyl)-1 H-benzoimidazol-2-yl]-4-hydroxy-piperidine (0.15 g, 0.46 mmol), and potassium carbonate (0.16 g, 1.13 mmol) in tetrahydrofuran/water (3/1) (40 mL). Heat to reflux. After 6 days, cool and evaporate in vacuo to obtain a residue. Partition the residue between dichloromethane and water. Extract the organic layer with 1 M hydrochloric acid solution, a 5% sodium bicarbonate solution, and water. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting sequentially with 10/1 ethyl acetate/methanol and 2/1 ethyl acetate/methanol to give the title compound: Rf=0.57 (silica gel, 2/1 ethyl acetate/methanol).

1. temperatureHeat to reflux
2. temperaturecool
3. customevaporate in vacuo
4. customto obtain a residue
5. customPartition the residue between dichloromethane and water
6. extractionExtract the organic layer with 1 M hydrochloric acid solution
7. dry with materialDry the organic layer over Na2SO4
8. filtrationfilter
9. concentrationconcentrate in vacuo
10. customto obtain a residue