化学合成。
化学合成
合成路线 1(1. 合成:28165-52-8)
产率:41%
合成条件:Stage #1: at 0℃; Stage #2: for 1 h; Heating / reflux
实验步骤:在0℃下,将亚硝酸钠(65.2mmol)分几批加入到2,5-二溴苯胺(55.8mmol)的三氟乙酸(80mL)溶液中。 将所得溶液加入到50%硫酸(120mL)中的硫酸钠(10g)的沸腾溶液中,并将反应混合物保持回流1小时。 然后将产物蒸汽蒸馏,用二氯甲烷(2×200mL)萃取馏出物。 将合并的有机层干燥(硫酸钠)并浓缩,得到2,5-二溴苯酚,41%收率,为黄色固体。
参考文献:
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