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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
【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.
【Key words】 time-resolved fluorescence immunoassay(TRFIA); 4-bromo-2,6-bis(3-(bromomethyl)-1H-pyrazol-1-yl)pyridine; 4-bromo-2-(3-(bromomethyl)-1H-pyrazol-1-yl)-6-(3-methyl-1H-pyrazol-1-yl)pyridine; chelate;
- 【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