稳定同位素标记3,3’,4,4’-四氯联苯-D_(6)的合成及表征  

Synthesis and Characterization of Stable Isotope Labeled 3,3',4,4'-Tetrachlorobiphenyl-D_(6)

作　　者：汪榕 郭会 陈武炼 WANG Rong;GUO Hui;CHEN Wulian(Anpel Laboratory Technologies(Shanghai)Inc.,Shanghai 201600,China)

机构地区：[1]上海安谱实验科技股份有限公司,上海201600

出　　处：《同位素》2025年第2期185-190,共6页Journal of Isotopes

基　　金：基础科研条件与重大科学仪器设备研发重点专项(2021YFF0701902);上海市2021年度“科技创新行动计划”启明星项目(21QB1400800)。

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-D_(6)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-D_(6)(PCB 77-D_(6))。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(^(1)H-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。A new synthetic method of the stable isotope labeled 3,3',4,4'-tetrachlorobiphenyl-D_(6) was investigated.The synthesis of 3,3',4,4'-tetrachlorobiphenyl-D_(6) is based on 1,2-dichlorobenzene-D_(4) as the labeling precursor through three steps of catalyzed borylation,iodination,Suzuki coupling reaction.According to the amount of 1,2-dichlorobenzene-D_(4),the yield of 3,3',4,4'-tetrachlorobiphenyl-D_(6) was 72.85%.The structure of the target product was characterized by ^(1)H-NMR,gas-mass spectrometry and gas chromatography.The chemical purity of 3,3',4,4'-tetrachlorobiphenyl-D_(6) 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.

关 键 词：多氯联苯 稳定同位素标记 同位素内标 

分 类 号：TL99[核科学技术—核技术及应用] O628.1[理学—有机化学]