稳定同位素标记3,3’,4,4’-四氯联苯-D<sub>6</sub>的合成及表征

稳定同位素标记3,3’,4,4’-四氯联苯-D₆的合成及表征

摘要: 为建立一种合成稳定同位素标记的3,3’,4,4’-四氯联苯-D₆的新方法用于同位素内标，本研究以氘代邻二氯苯为原料，经催化硼化、碘化、Suzuki偶联共三步反应得到稳定同位素氘标记的3,3’,4,4’-四氯联苯-D₆(PCB 77-D₆)。结果表明，以氘代邻二氯苯计，本合成路线总收率为72.85%。通过核磁共振氢谱(¹H-NMR)、气相-质谱（GC-MS）和气相色谱(GC)等表征确认其结构，所得产品化学纯度为99.54%，同位素丰度为98.38 atom%D，可作为同位素内标用于多氯联苯的定性、定量检测。

Abstract: A new synthetic method of the stable isotope labeled 3,3',4,4'-tetrachlorobiphenyl-D₆ was investigated. The synthesis of 3,3',4,4'-tetrachlorobiphenyl-D₆ is based on 1,2-dichlorobenzene-D₄ as the labeling precursor through three steps of catalyzed borylation, iodination, Suzuki coupling reaction. According to the amount of 1,2-dichlorobenzene-D₄, the yield of 3,3',4,4'-tetrachlorobiphenyl-D₆ was 72.85%. The structure of the target product was characterized by ¹H-NMR, gas-mass spectrometry and gas chromatography. The chemical purity of 3,3',4,4'-tetrachlorobiphenyl-D₆ was 99.54%, and the abundance of deuterium isotope was 98.38 atom%D. It can be used as the isotope internal standard for the determination of polychlorinated biphenyls.