反应详情

温度

80 °C

Combine (1H-benzimidazol-2-yl)(1-(t-butoxycarbonyl)piperidin-4-yl)amine (0.51 g, 1.61 mmol) and dimethylformamide (15 mL). Add sodium hydride (0.086 g, 60% in oil, 2.15 mmol). Heat to 80° C. After 15 minutes, add ethyl 4-bromobutyrate (0.35 mL, 2.45 mmol) and continue heating at 80° C. After 18 hours, cool and partition the reaction mixture between dichloromethane and a saturated aqueous sodium bicarbonate solution. Separate the layers and extract the organic layer with brine. Dry the organic layer over MgSO4, filter, and concentrate in vacuo to give (1-(3-carboethoxypropyl)-1H-benzimidazol-2-yl)(1-(t-butoxycarbonyl)piperidin-4-yl)amine.

1. temperaturecontinue heating at 80° C
2. waitAfter 18 hours
3. temperaturecool
4. custompartition the reaction mixture between dichloromethane
5. customSeparate the layers
6. extractionextract the organic layer with brine
7. dry with materialDry the organic layer over MgSO4
8. filtrationfilter
9. concentrationconcentrate in vacuo