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对两种不同体系下合成4-溴-4’碘联苯进行了研究。通过对比发现,浓硫酸做催化剂,I2/KIO4为碘化试剂的反应体系具有可行性。对该体系的反应温度和浓硫酸的用量进行了优化。原料4溴联苯,在浓硫酸催化下,与碘/碘酸钾在冰醋酸水溶液中,于100℃下反应2h,紫色褪尽,过滤得到白色固体粗品34g,纯度98%(HPLC),收率为95%。该方法降低了原料成本,简化操作,缩短反应时间,是较为理想4-溴-4’碘联苯的工业合成方法。
The synthesis of 4-bromo-4’-iodobiphenyl under two different systems was studied. By contrast, it is feasible to use concentrated sulfuric acid as catalyst and I2 / KIO4 as iodination reagent. The reaction temperature and the amount of concentrated sulfuric acid were optimized. The raw material 4bromobiphenyl was reacted with iodine / potassium iodate in glacial acetic acid aqueous solution under the catalysis of concentrated sulfuric acid for 2h at 100 ℃. The purple color faded out and the white solid crude product was filtered to obtain 34g with a purity of 98% (HPLC). The rate is 95%. The method reduces the raw material cost, simplifies the operation and shortens the reaction time, and is an ideal industrial synthesis method of 4-bromo-4’-iodobiphenyl.