反应详情

温度

23 °C

To a suspension of ethyl (2E)-3-[6-(4-piperidylamino)-3-pyridyl]acrylate dihydrochloride (500 mg) in DMF (5 ml) was added 4-(1H-pyrrol-1-yl)benzoic acid (309 mg), EDCI.HCl (317 mg), HOBt (223 mg), Et3N(0.63 ml), the mixture was stirred at 23° C. for 8 hours. The mixed solution was poured into a mixture of water (20 ml) and AcOEt (20 ml). The organic layer was separated, washed with water twice and brine, dried-over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluted with 5% MeOH in dichloromethane to give ethyl (2E)-3-[6-({1-[4-(1H-pyrrol-1-yl)benzoyl]-4-piperidyl}amino)-3-pyridyl]acrylate (686 mg).

1. customThe organic layer was separated
2. washwashed with water twice
3. concentrationbrine, dried-over sodium sulfate and concentrated in vacuo
4. customThe residue was purified by silica gel column chromatography
5. washeluted with 5% MeOH in dichloromethane