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) (1.51 g, 3.2 mmol), 4-(1-(4-fluorobenzyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic acid salt (1.78 g, 3.07 mmol), and triethylamine (2 mL, 14.35 mmol) in acetonitrile (40 mL). Heat to reflux. After 22 hours, cool to ambient temperature and dilute with dichloromethane, and extract with a saturated aqueous sodium bicarbonate solution and then brine. Dry the organic layer over MgSO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with dichloromethane/methanol/concentrated ammonium hydroxide 95/5/0.05 to give the title compound.

1. temperatureHeat to reflux
2. extractionextract with a saturated aqueous sodium bicarbonate solution
3. dry with materialDry the organic layer over MgSO4
4. filtrationfilter
5. customevaporate in vacuo
6. customto give a residue