反应详情

Combine 1-ethoxycarbonyl-4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (17.2 g, 47.6 mmol), hydrazine hydrate (40 mL), and potassium hydroxide (40.7 g, 725 mmol) in ethylene glycol (150 mL). Heat to reflux. After 5 hours, cool the reaction mixture and dilute with water (500 mL). Extract three times with dichloromethane. Combine the dichloromethane layers 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 the title compound: Rf=0.25 (silica gel, dichloromethane/methanol, 90/10).

1. temperatureHeat to reflux
2. temperaturecool the reaction mixture
3. extractionExtract three times with dichloromethane
4. extractionextract with a saturated aqueous sodium bicarbonate solution
5. dry with materialDry the organic layer over MgSO4
6. filtrationfilter
7. customevaporate in vacuo