反应详情

Combine 1-(3,4,5-trimethoxy-benzoyl)-3-(3,4-dimethoxy-phenyl)-3-(2-methanesulfonyl-ethyl)-pyrrolidine (0.69 g, 1.32 mmol) and 4-[1-(4-fluoro-benzyl)-1 H-benzoimidazole-2-carbonyl]-piperidine (0.49 g, 1.42 mmol), and sodium bicarbonate (0.223 g, 2.64 mmol) in tetrahydrofuran/water (15/4) (30 mL). Heat to reflux. After 72 hours, cool and evaporate in vacuo to obtain a residue. Partition the residue between dichloromethane and 5% sodium bicarbonate solution. Dry the organic layer over MgSO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 5/1 ethyl acetate/methanol to give an oil. Combine the oil with dichloromethane and extract with 5% sodium bicarbonate solution. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Dry the residue in vacuo at 82° C. to give the title compound: Rf=0.27 (silica gel, 5/1 ethyl acetate/methanol); mp; 80-83° C. Elemental Analysis calculated for C44H49FN4O7: C 69.09; H 6.46; N 7.32; Found: C 68.82; H 6.44; N 7.42.

1. temperatureHeat to reflux
2. temperaturecool
3. customevaporate in vacuo
4. customto obtain a residue
5. customPartition the residue between dichloromethane and 5% sodium bicarbonate solution
6. dry with materialDry the organic layer over MgSO4
7. filtrationfilter
8. concentrationconcentrate in vacuo
9. customto obtain a residue
10. extractionextract with 5% sodium bicarbonate solution
11. dry with materialDry the organic layer over Na2SO4
12. filtrationfilter
13. concentrationconcentrate in vacuo
14. customto obtain a residue
15. customDry the residue in vacuo at 82° C.