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双格氏试剂法合成4,4’-二(二苯基膦基)联苯

Synthesis of 4,4'-bis(diphenylphosphine) biphenyl via di-Grignard reagent
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摘要 以4-溴联苯为原料,通过卤代反应获得二溴联苯后,与活泼金属镁反应制备双格氏试剂,再与二苯基氯化磷反应一步合成目标化合物4,4’-二(二苯基膦基)联苯.采用核磁共振谱(1H、13C、31P NMR)、傅里叶变换红外光谱(FT-IR)、液质联用飞行时间质谱(LC-MS TOF)等对目标化合物进行表征,表征结果与结构相吻合.与传统的合成法相比,该法具有操作简便、反应条件温和、原料成本低等优点. Organic disphosphine compounds have attracted great attention due to their unique properties.By halogenation with 4-bromobiphenyl,dibromobiphenyl was obtained and further reacted with magnesium to prepare di-Grignard reagent,then reacted with chlorodiphenylphosphine,the title compound 4,4'-bis(diphenylphosphine) biphenyl was synthesized.And the structure of the title compound was characterized and confirmed by (1H, 13C and 31p) NMR, FT-IR and LC-MS TOF.Compared with traditional synthesis method, this method has advantages of simple operation, mild reaction condition and low material cost.
出处 《湖北大学学报(自然科学版)》 CAS 2015年第4期387-390,共4页 Journal of Hubei University:Natural Science
基金 湖北省自然科学基金(2013CFA087)资助
关键词 4 4’-二(二苯基膦基)联苯 双格氏试剂 合成 表征 4,4' -bis(diphenylphosphine)biphenyl di-Grignard reagent synthesis characterization
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