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

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。

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-lH-pyrazol-1-yl） pyridine by diazotizing reaction and brominating reaction. The structure of the product was determined by IR,^1 HNMR,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）-lH-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.