胸腺嘧啶-^(15)N_2的合成与表征

Synthesis and Characterization of Thymine-^(15)N_2

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-15 N2缩合,在甲醇钠作用下环化反应得到胸腺嘧啶-15 N2。合成方法操作简单,工艺流程短,副产物少,收率可达80%,15 N同位素丰度稳定。产物经HPLC、IR、MS、1 H NMR和13 C NMR表征,结果表明:产物化学纯度>99%,15 N同位素丰度>98atom%。

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 15 N abundance did not diluted.The product was characterized by HPLC,IR,MS,1 H NMR and 13 C NMR.The chemical purity was more than 99%and15 N enrichment was more than 98atom%.