反应 #1255619
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09428496B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Ethyl 4-(5-hydroxypentyl)piperazinecarboxylate (10.87 g, 65.09 mmol), 10% aqueous sodium hydroxide solution (150 mL) and ethanol (150 mL) were placed in a 500 mL round-bottomed flask, and heated under reflux with stirring overnight; the reaction system was cooled down to room temperature, and the solvent was distilled off under reduced pressure, to obtain a pale yellow oil; to the oil, 200 ml of saturated brine was added, followed by extraction with dichloromethane (5×200 mL); the resulting extract was dried with Na2SO4, filtered, and concentrated to obtain a pale yellow oil 9.69 g, yield 86.5% (which was directly used in the next step reaction). heated under reflux the solvent was distilled off under reduced pressure to obtain a pale yellow oil followed by extraction with dichloromethane (5×200 mL) the resulting extract was dried with Na2SO4 filtered concentrated
来源 ID: ord-f80d50f7da2b46d5a86aeaf9c80fcb3a