反应详情

Combine 1-(2-methoxy-5-(1H-tetrazol-1-yl)benzoyl)-3-phenyl-3-(2-methanesulfonyloxyethyl)pyrrolidine (prepared from (−)-3-phenyl-3-(2-hydroxyethyl)pyrrolidine(R,R)-di-p-anisoyltartaric acid salt) (0.93 g, 1.97 mmol), 4-(1-(2-methoxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic acid salt (1.04 g, 1.97 mmol), and triethylamine (1.5 mL, 10.76 mmol) in acetonitrile (20 mL). Heat to reflux. After 18 hours, cool and partition the reaction mixture between brine and dichloromethane. Dry the organic layer over MgSO4, filter, and evaporate in vacuo to give residue. Chromatograph the residue on silica gel eluting with dichloromethane/methanol/concentrated aqueous ammonia 95/5/0.05 to give the title compound: Rf=0.49 (silica gel, dichloromethane/methanol/concentrated aqueous ammonia 95/5/0.1).

1. temperatureHeat to reflux
2. temperaturecool
3. custompartition the reaction mixture between brine and dichloromethane
4. dry with materialDry the organic layer over MgSO4
5. filtrationfilter
6. customevaporate in vacuo
7. customto give residue