反应 #1073489
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07199147B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 1-benzyl-4-azepanone (610 mg, 3.00 mmol) in diethyl ether (8 ml) was added to a suspension of lithium aluminum hydride (57 mg, 1.50 mmol) in diethyl ether (5 ml) at 0° C. and stirred for 1 hour. Water (0.057 ml), a 2N-aqueous sodium hydroxide solution (0.114 ml) and then water (0.171 ml) were added to the reaction mixture, and the resulting mixture was dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate 1/1, chloroform/methanol=30/1) to obtain 1-benzyl-4-azepanol (516 mg, 84%). the resulting mixture was dried over anhydrous magnesium sulfate distilled under reduced pressure to remove the solvent The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate 1/1, chloroform/methanol=30/1)
来源 ID: ord-c771e64275094d2ab2cd2bf462e7766e