13C1-对乙酰氨基酚（-CO13CH3）的合成及结构表征

Synthesis and Structure Characterization of 13C1-Paracetamol（-CO13CH3）

摘要:

2-13C1-乙酸与N,N'-羰基二咪唑反应得到了中间体13C1-N-乙酰基咪唑（—CO13CH3），该中间体进一步与对氨基苯酚反应得到13C1-对乙酰氨基酚（—CO13CH3）。考察了反应温度和反应时间两个因素对13C1-对乙酰氨基酚收率的影响。结果表明，合成产物的最佳反应温度和时间分别为40 ℃和12 h。产物经GC-MS、FTIR、1HNMR和13CNMR进行结构表征及含量测定。化学纯度>99%，同位素丰度>98.7%，总产率为87%，标记合成的产物可作为同位素内标物在定量分析测试中使用。

Abstract:

13C1-N-Acetylimidazole (—CO13CH3) was synthesized by reacting 2-13C1-acetic acid with N,N'-carbonyldiimidazole, and then reacted with p-aminophenol to obtain 13C1-paracetamol (—CO13CH3). The influences of factors such as temperature and reaction time on the yield of products were investigated. The results showed that the optimal reaction temperature and time for the product synthesis were 40 ℃ and 12 h, respectively. The product was characterized by GC-MS, FTIR, 1HNMR and 13CNMR. The results showed that paracetamol contained one 13C atoms. The chemical purity was better than 99% and 13C enrichment was more than 98.7 atom%. The yield of product was 87%. Synthetic product can be used as an isotope internal standard in quantitative analysis testing.