反应详情

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(3,4-dimethoxyphenyl)-3-(2-methanesulfonyloxyethyl)pyrrolidine (0.51 g, 0.97 mmol) and (1-(2-ethoxyethyl)-1H-benzimidazol-2-yl)(piperidin-4-yl)amine (0.34 g, 1.2 mmol), and N,N-diisopropylethylamine (0.25 g, 1.9 mmol) in acetonitrile (5 mL). Heat to reflux. After 54 hours, partition the residue between ethyl acetate and 5% sodium bicarbonate solution. Separate the layers and extract the organic layer with 5% sodium bicarbonate and then water. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 1/1 ethyl acetate/methanol to give a residue. Combine the residue with dichloromethane and extract with water. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Dry the residue in vacuo at 60° C. to give the title compound: Rf=0.37 (silica gel, 1/1 ethyl acetate/methanol).

1. temperatureHeat to reflux
2. custompartition the residue between ethyl acetate and 5% sodium bicarbonate solution
3. customSeparate the layers
4. extractionextract the organic layer with 5% sodium bicarbonate
5. dry with materialDry the organic layer over Na2SO4
6. filtrationfilter
7. concentrationconcentrate in vacuo
8. customto obtain a residue
9. extractionextract with water
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 60° C.