反应详情

Combine (1-(fur-2-ylmethyl)-1H-benzimidazol-2-yl)(1-(ethoxycarbonyl)piperidin-4-yl)amine (1.38 g, 3.75 mmol), potassium hydroxide (3.0 g, 56.1 mmol) in ethylene glycol (15 mL). Add hydrazine hydrate (3.09 mL, 63.7 mmol). Heat to reflux. After 18 hours, cool, add water, and extract four times with dichloromethane (200 mL). Combine the organic layers, dry over MgSO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with sequentially with ethyl acetate, 25% methanol/ethyl acetate, 50% methanol/ethyl acetate, 75% methanol/ethyl acetate, and then methanol to give a residue. Dissolve the residue in dichloromethane, extract with water and then brine, dry over MgSO4, filter, and evaporate in vacuo to give the title compound.

1. temperatureHeat to reflux
2. temperaturecool
3. extractionextract four times with dichloromethane (200 mL)
4. dry with materialCombine the organic layers, dry over MgSO4
5. filtrationfilter
6. concentrationconcentrate in vacuo
7. customto obtain a residue
8. extractionextract with water
9. dry with materialbrine, dry over MgSO4
10. filtrationfilter
11. customevaporate in vacuo