反应详情

Combine 1-benzoyl-3-(3,4-dimethoxy-phenyl)-3-(2-methanesulfonyl-ethyl)-pyrrolidine (0.20 g, 0.46 mmol) and 4-(benzothiazole-2-carbonyl)-piperidine (0.11 g, 0.46 mmol), and sodium carbonate (0.098 g, 0.92 mmol) in tetrahydrofuran/water (15/4) (30 mL). Heat to reflux. After 4 days, cool to ambient temperature and evaporate in vacuo to obtain a residue. Partition the residue between dichloromethane and 5% sodium bicarbonate solution. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 10/1 ethyl acetate/methanol to give a residue. Combine the solid 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=0.21 (silica gel, 10/1 ethyl acetate/methanol); mp; 74-76° C.

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