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TRFIA螯合剂中间体2,6-二(3′-溴甲基-1′-吡唑基)-4-溴吡啶的合成、分离与表征

Synthesis,Separation and Characterization of TRFIA Chelates Intermediate 4-Bromo-2,6-bis(3-(bromomethyl)-1H-pyrazol-1-yl)pyridine

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【作者】 刘婷婷宁志刚赫文龙潘利华

【Author】 LIU Ting-ting1,NING Zhi-gang1,HE Wen-long1,PAN Li-hua2(1.Institute of Bioengineering,Changchun University of Technology,Changchun 130012,China;2.National Analytical Research Center of Electrochemistry and Spectroscopy,Changchun Institute of Applied Chemistry,Chinese Academy of Science,Changchun 130022,China)

【机构】 长春工业大学生物工程学院中国科学院长春应用化学研究所国家电化学光谱分析研究中心

【摘要】 以2,6-二(3-甲基-1-H-吡唑基)-4-溴吡啶为原料,经重氮化、溴化合成了新型时间分辨荧光免疫分析(TR-FIA)双功能螯合剂中间体2,6-二(3′-溴甲基-1′-吡唑基)-4-溴吡啶,通过IR、GC-MS1、HNMR和元素分析等对其结构进行了确认,探讨了合成条件及反应机理。同时,通过GC-MS1、HNMR和元素分析等对第一副产物4-溴-2-(3′-溴甲基-1′-吡唑基)-6-(3′-甲基-1′-吡唑基)吡啶的结构也进行了确认,以其为原料可继续合成目标化合物,大幅提高总产率。

【Abstract】 A new bifunctional chelate intermediate of time-resolved fluorescence immunoassay 4-bromo-2,6-bis(3-(bromomethyl)-1H-pyrazol-1-yl)pyridine was prepared from 4-bromo-2,6-bis(3-methyl-1H-pyrazol-1-yl)pyridine by diazotizing reaction and brominating reaction.The structure of the product was determined by IR,1HNMR,GC-MS and elemental analysis.The reaction conditions and reaction mechanism were also researched.At the same time,the main outgrowth 4-bromo-2-(3-(bromomethyl)-1H-pyrazol-1-yl)-6-(3-methyl-1H-pyrazol-1-yl)pyridine was separated and its structure was determined by 1HNMR,GC-MS and elemental analysis as well.And the target product could also be prepared from it,so the yield was increased greatly.

【基金】 国家自然科学基金资助项目(30471606)
  • 【文献出处】 化学与生物工程 ,Chemistry & Bioengineering , 编辑部邮箱 ,2009年06期
  • 【分类号】O626.32
  • 【被引频次】1
  • 【下载频次】98
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