~(13)C,~(15)N_3-盐酸氨基脲合成方法的优化

采用13C,15N2双标记尿素和15N2标记水合肼为原料,经回流反应一步合成13C,15N3-盐酸氨基脲。通过单因素考察和正交实验对13C,15N3-盐酸氨基脲的合成工艺进行优化,得到最优反应条件为:15N2-水合肼与13C,15N2-尿素的进料摩尔比为1.4∶1,加热温度为135℃,反应时间为4.5 h。采用此优化合成条件单步合成反应收率90%,13C,15N3-盐酸氨基脲纯度≥98%,13C丰度≥97%,15N丰度≥99%。结果显示,该方法具有反应周期短,产物收率高,后处理简便易行等优点。

Study on Synthesis of 13C, 15N3-Semicarbazide Hydrochloride

The ^13C,^15N2 doubly labeled Urea and 15N2 labeled Hydrazine hydrate were used as raw materials,and ^13C,^15N3-SEM·HCl was synthesized by a direct one-step synthesis which based on the reflux reacting.The reaction conditions of ^13C,^15N3 labeled semicarbazide hydrochloride were mainly investigated by the experiment designs,like single-factor design and orthogonal design.The following optimized conditions were obtained as follow： the mole ratio ^15N2-N2H4 to ^13C,^15N2-urea was 1.4∶1,the reaction temperature was 135 ℃,the reaction time was 4.5 h,and the yield of ^13C,^15N3 labeled semicarbazide hydrochloride was above 90%,the purity ≥98%,the abundance of 13C ≥97%,the abundance of 15N ≥99%.This technology had many advantages,like short production cycle,high yield and sample later-processing.