化学合成。
化学合成
合成路线 1(1. 合成:1646-54-4)
产率:95%
合成条件:With bromine; iodine In dichloromethane at 50℃; for 3 h; Darkness; Inert atmosphere
实验步骤:在氮气气氛下,在反应器中向搅拌器(150ml,带有漏斗,冷凝器和氮气入口)中加入4颈用于1,2,4,5-四甲基苯(Aldrich Co.),然后在圆底烧瓶中充分干燥,加入8.0克0.124克碘,加入23.84毫升二氯甲烷,搅拌至完全溶解。使用加料漏斗将反应溶液加到溴上,在22.86ml中2小时。此时,溴在给定条件下反应,整个反应器包裹在铝箔中,从外部吸收光线,以防止由于光引起的副反应。反应加入后的反应混合物在50℃下完成1小时,并通过向烧瓶中加入少量5N氢氧化钠水溶液以除去未反应的溴。在分液漏斗中将有机层的下部转移到所得有机层与水溶液的混合物中。将它们分离。通过加入硫酸镁除去少量剩余的水,过滤,分离有机层,二氯甲烷作为溶剂,通过重结晶得到纯白色晶体。 60将它们在真空烘箱中干燥6小时,得到目标化合物3',6-二溴-1,2,4,5-四甲基苯:得到(16.53g,95%收率)。
参考文献:
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