反应 #2175213
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05814634
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 1-(2-aminoethyl)piperidine(5.01 g) in dichloromethane (100 ml) were added triethylamine(11 ml) and acetic anhydride(4.4 ml) and then the mixture was stirred at room temperature for 40 minutes. The reaction solution was washed with saturated sodium hydrogencarbonate aqueous solution and saturated brine successively, dried over sodium sulfate anhydride, and concentrated under a vacuum. The residue was dropped into a suspension of lithium aluminium hydride (3.46 g) in tetrahydrofuran(100 ml). After being refluxed with heating for 1 hour, the reaction mixture was filtrated. The filtrate was concentrated, thereby yielding 4.43 g(79%) of 1-[2-(ethylamino)ethyl]piperidine. The reaction solution was washed with saturated sodium hydrogencarbonate aqueous solution and saturated brine successively dried over sodium sulfate anhydride concentrated under a vacuum The residue was dropped into a suspension of lithium aluminium hydride (3.46 g) in tetrahydrofuran(100 ml) After being refluxed with heating for 1 hour the reaction mixture was filtrated The filtrate was concentrated
来源 ID: ord-6cb8a8411d704825b480ef9b8c3f7f7f