反应详情

1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide-hydrochloide (1.34 g, 7 mmol), anhydrous 1-hydroxybenzotriazole (0.95 g, 7 mmol), triethylamine(1.0 ml, 7.5 mmol) and N-methylpiperazine (664 μl, 6 mmol) were added to a mixture of [3-(2-formyl-4,5,6,7-tetrahydro-1H-indol-3-yl)-propionic acid] (1.1 g, 5 mmol) in 20 ml of N,N-dimethylformamide. The reaction was stirred at room temperature overnight. Thin layer chromatography (methanol: dichloromethane 5:1) showed one major spot. The reaction solution was concentrated under high vacuum over night then the residue was purified by flash chromatography and eluting with (dichloromethane: methanol 15/1, 10/1, 5/1) to give 3-[3-(4-methyl-piperazin-1-yl)-3-oxo-propyl]-4,5,6,7-tetrahydro-1H-indole-2-carbaldehyde (1.18 g, 78% yield).

1. concentrationThe reaction solution was concentrated under high vacuum over night
2. customthe residue was purified by flash chromatography
3. washeluting with (dichloromethane: methanol 15/1, 10/1, 5/1)