反应详情

温度

72.5 °C

Combine 1-(3,4,5-trimethoxy-benzoyl)-3-(3,4-dimethoxy-phenyl)-3-(2-methanesulfonyl-ethyl)-pyrrolidine (0.70 g, 1.3 mmol) and 4-[1-(4-fluoro-benzyl)-1 H-benzoimidazol-2-yl]-4-hydroxy-piperidine (0.58 g, 1.8 mmol), and potassium carbonate (0.37 g, 2.7 mmol) in dimethylformamide (22 mL). Heat to 70-75° C. After 4 days, cool and evaporate in vacuo to obtain a residue. Partition the residue between ethyl acetate and water. Extract the organic layer with water and a saturated solution of potassium carbonate. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 2/1 ethyl acetate/methanol to give a foam. Combine the foam with dichloromethane and extract with 5% sodium bicarbonate solution. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain the title compound: Rf=0.37 (silica gel, 2/1 ethyl acetate/methanol); mp; 110-120° C.

1. temperaturecool
2. customevaporate in vacuo
3. customto obtain a residue
4. customPartition the residue between ethyl acetate and water
5. extractionExtract the organic layer with water
6. dry with materialDry the organic layer over Na2SO4
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