13C1-对乙酰氨基酚(-CO13CH3)的合成及结构表征
DOI:
作者:
作者单位:

作者简介:

通讯作者:

中图分类号:

基金项目:

国家重点研究发展计划(批准号:2016YFD0200201)和国家自然科学基金(批准号:31772175和31621064)。


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

Fund Project:

The National Key Research and Development Program of China (Grant No. 2016YFD0200201) and The National Natural Science Foundation of China (Grant No. 31772175 and 31621064).

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 资源附件
  • |
  • 文章评论
    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.

    参考文献
    相似文献
    引证文献
引用本文

全海源,王智楠,吴长才,梅向东,宁君,折冬梅.13C1-对乙酰氨基酚(-CO13CH3)的合成及结构表征[J].精细化工,2020,37(8):

复制
分享
文章指标
  • 点击次数:
  • 下载次数:
  • HTML阅读次数:
  • 引用次数:
历史
  • 收稿日期:2019-11-04
  • 最后修改日期:2020-02-15
  • 录用日期:2020-02-18
  • 在线发布日期: 2020-06-30
  • 出版日期: