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以对甲氧基联苯胺为原料,在-5~0℃下进行重氮化,再与氯化亚铜或溴化亚铜在90℃发生Sandmeyer反应,得到4-甲氧基-3-卤代联苯,考察了原料配比、反应温度和反应时间等对反应的影响,并通过熔点、红外光谱、核磁共振波谱等对其进行了表征。研究结果表明,采用该方法合成的3-氯-4-甲氧基联苯的总收率为63%,3-溴-4-甲氧基联苯的总收率为51%。
4-Methoxy-3-halogenated biphenyl was synthesized from p-dimethoxybenzidine via diazotization at -5～0℃ and Sandmeyer reaction with cuprous bromide or cuprous chloride at 90℃,some factors affected the reaction, such as the material ratio, the reaction time and temperature were discussed. The structure of the product was confirmed by melting point, IR and ~1HNMR.The resultsshow that the total yield of 3-chloro-4-methoxybiphenyl synthesized by this preparation procedure was 63% and 3-bromo-4-methoxybiphenyl was 51%.
