反应详情

Combine 1-(3,4,5-trimethoxybenzoyl)-3-phenyl-3-(2-methanesulfonyloxyethyl)pyrrolidine (0.34 g, 0.72 mmol), 4-(1-(2-(1H-tetrazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic acid salt (0.41 g, 0.72 mmol), and N,N-diisopropylethylamine (0.33 g, 2.53 mmol) in acetonitrile (10 mL). Heat to reflux. After 12 hours, cool to ambient temperature and dilute the reaction mixture with dichloromethane and extract with twice water. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 5% methanol/dichloromethane/0.5% concentrated aqueous ammonia). Combine the product containing fractions, evaporate in vacuo, dissolve in dichloromethane, and extract with water, dry over Na2SO4, filter, and evaporate in vacuo to to give the title compound: Rf=0.30 (silica gel, 5% methanol/dichloromethane/0.5% concentrated aqueous ammonia).

1. temperatureHeat to reflux
2. extractionextract with twice water
3. dry with materialDry the organic layer over Na2SO4
4. filtrationfilter
5. customevaporate in vacuo
6. customto give a residue
7. additionCombine the product containing fractions
8. customevaporate in vacuo
9. dissolutiondissolve in dichloromethane
10. extractionextract with water
11. dry with materialdry over Na2SO4
12. filtrationfilter
13. customevaporate in vacuo