JOURNAL OF ISOTOPES

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Synthesis and Characterization of Thymine-15N2

XU Jian-fei;DU Xiao-ning;WANG Wei;LEI Wen;HOU Jie   

  1. Research Institute of Isotope, Shanghai Research Institute of Chemical Industry, Shanghai 200062, China
  • Online:2016-02-20 Published:2016-03-01

胸腺嘧啶-15N2的合成与表征

徐建飞;杜晓宁;王伟;雷雯;侯捷   

  1. 上海化工研究院 同位素研究所,上海200062

Abstract:

A novel and mild synthesis method of thymine-15N2 was designed. Ethyl formate and ethyl propionate as raw materials, the intermediate ethyl 2-formylpropionate was condensed under sodium metal, the target compound thymine-15N2 was obtained by condensation with isotope urea-15N2 under acid catalysis. Synthesis route had the advantages of simple operation, short process flow and less side product. The yield was more than 80% and isotope 15N abundance did not diluted. The product was characterized by HPLC, IR, MS, 1H NMR and 13C NMR. The chemical purity was more than 99% and 15N enrichment was more than 98 atom%.

Key words: isotope, thymine, ethyl 2-formylpropionate

摘要:

以甲酸乙酯和丙酸乙酯为原料,在金属钠存在下缩合得到中间体2-甲酰丙酸乙酯,中间体在酸催化下与同位素尿素-15N2缩合,在甲醇钠作用下环化反应得到胸腺嘧啶-15N2。合成方法操作简单,工艺流程短,副产物少,收率可达80%,15N同位素丰度稳定。产物经HPLC、IR、MS、1H NMR和13C NMR表征,结果表明:产物化学纯度>99%,15N同位素丰度>98 atom%。

关键词: 同位素, 胸腺嘧啶, 2-甲酰丙酸乙酯