反应 #1074521
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07202364B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of N-(6-acetyloxy-1-chloro-2-naphthyl)carbamic acid ethyl ester (375 mg, 1.34 mmol) and KOH (903 mg, 16.1 mmol) in ethanol (10 mL) is heated to reflux temperature under N2 atmosphere for 4.5 hours. The reaction mixture is concentrated by rotary evaporator under high vacuum. The residual oil is partitioned between EtOAc and water. After acidification (2 N HCl), the organic layer is separated, washed with brine and dried (MgSO4). Concentration by rotary evaporator gives 1-chloro-2-amino-6-naphthol as a brown solid. is heated to reflux temperature under N2 atmosphere for 4.5 hours The reaction mixture is concentrated by rotary evaporator under high vacuum The residual oil is partitioned between EtOAc and water After acidification (2 N HCl), the organic layer is separated washed with brine dried (MgSO4) Concentration by rotary evaporator
来源 ID: ord-365afdb2b5404602b96f2812f7729d22