对乙酰氨基酚-2-^13C的合成及表征  

Synthesis and characterization of paracetamol-2-C

作　　者：全海源 王智楠 吴长才 宁君[1] 梅向东[1] 折冬梅[1] QUAN Haiyuan;WANG Zhinan;WU Changcai;NING Jun;MEI Xiangdong;SHE Dongmei(Institute of Plant Protection,Chinese Academy of Agricultural Sciences,Beijing 100193,China)

机构地区：[1]中国农业科学院植物保护研究所,北京100193

出　　处：《精细化工》2020年第8期1724-1728,共5页Fine Chemicals

基　　金：国家重点研究发展计划(2016YFD0200201);国家自然科学基金(31772175、31621064)。

摘　　要：以乙酸-2-^13C与N,N’-羰基二咪唑为原料,反应得到中间体N-乙酰基咪唑-2-^13C,该中间体进一步与对氨基苯酚反应得到对乙酰氨基酚-2-^13C。考察了反应温度和反应时间对对乙酰氨基酚-2-^13C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12h。产物经GC-MS、FTIR、1HNMR和^13CNMR进行结构表征。对乙酰氨基酚-2-^13C的气相色谱纯度>99%,同位素丰度为98.7%,总产率为87%,合成的产物可作为同位素内标物在定量分析测试中使用。N-Acetylimidazole-2-^13C was prepared from acetic acid-2-^13C with N,N’-carbonyldiimidazole.Subsequently,it reacted with p-aminophenol to give paracetamol-2-^13C.The factors affecting the yield of paracetamol-2-^13C,such as temperature and reaction time 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,1 HNMR and^13CNMR.It was found that the GC purity of N-acetylimidazole-2-^13C was greater than 99%,and^13C isotope abundance was 98.7%.The total yield of product was 87%.Therefore,the synthetic product can be used as an isotope internal standard in quantitative analysis testing.

关 键 词：乙酸-2-^13C N N’-羰基二咪唑 对乙酰氨基酚-2-^13C 同位素内标物 定量分析 精细化工中间体 

分 类 号：O628.21[理学—有机化学]