4,4′-二(羟甲基)联苯的合成  

Synthesis of 4,4′-bis(hydroxymethyl)biphenyl

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作  者:杨涛[1] 唐璇[1] 薛珊 周宛欣 成西涛[2] YANG Tao;TANG Xuan;XUE Shan;ZHOU Wanxin;CHENG Xitao(College of Chemistry and Chemical Engineering,Xi’an Shiyou University,Xi’an 710065,China;Shaanxi Petrochemical Research and Design Institute,Xi′an 710054,China)

机构地区:[1]西安石油大学化学化工学院,陕西西安710065 [2]陕西省石油化工研究设计院,陕西西安710054

出  处:《合成化学》2022年第9期697-703,共7页Chinese Journal of Synthetic Chemistry

基  金:2019陕西省工业攻关资助项目(2019SF-263);联苯二氯苄的水解工艺研究项目(YCS21213188)。

摘  要:以4,4′-二(氯甲基)联苯为原料,经水解生成苄醇类化合物4,4′-二(羟甲基)联苯。采用~1H NMR,IR,HPLC对产物进行了表征。研究讨论了反应条件、催化剂等因素对产物含量和收率的影响,并且优化了4,4′-二(羟甲基)联苯的合成工艺,提出了可能的催化反应机理。结果表明:聚乙二醇作为催化剂,可与溶液中的阳离子发生络合,增强了亲核试剂的反应活性,提高了反应速率。在优化工艺下反应12 h,粗产品HPLC含量可达97.2%,收率93.9%。Using 4,4′-bis(chloromethyl)biphenyl as raw material,it is hydrolyzed to generate benzyl alcohol compound-4,4′-bis(hydroxymethyl)biphenyl.The obtained product was characterized by ~1H NMR,IR,HPLC.The effects of the reaction conditions and catalysts on product content and yield were discussed.The synthesis process of 4,4′-bis(hydroxymethyl)biphenyl was optimized,and a possible reaction mechanism was proposed.The results show that polyethylene glycol as a catalyst,complexes with cations in the solution,enhancing the reaction reactivity of nucleophiles and improving the reaction rate.After 12 hours of reaction under the optimized conditions,the content of crude product reached 97.2% by HPLC,and the yield was 93.9%.

关 键 词:4 4′-二(氯甲基)联苯 4 4′-二(羟甲基)联苯 合成 表征 反应机理 

分 类 号:O625.34[理学—有机化学]

 

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