环磺酮原药中3个杂质结构的确定及其合成
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摘要
采用文献中报道的环磺酮的合成工艺合成了环磺酮原药,通过高效液相色谱分析,发现其原药中含有3个质量分数分别大于0.1%的杂质;通过核磁共振氢谱(1H NMR)及高分辨质谱(HRMS)对3个杂质的结构进行了确证,同时进行了合成。根据合成工艺路线,对该杂质产生的途径进行了分析。
Tembotrione was prepared according to the reported method. Three main impurities over 0.1% were detected by high-performance liquid chromatography(HPLC). The structures of those impurities were characterized by ~1H NMR and high resolution mass spectrometer(HRMS). Then the impurities were synthesized. The produced pathways of impurities were also analyzed according to the synthetic route.
Tembotrione was prepared according to the reported method. Three main impurities over 0.1% were detected by high-performance liquid chromatography(HPLC). The structures of those impurities were characterized by ~1H NMR and high resolution mass spectrometer(HRMS). Then the impurities were synthesized. The produced pathways of impurities were also analyzed according to the synthetic route.
引文
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[4]华乃震.三酮类除草剂产品及其应用[J].世界农药,2015,37(6):7-13.HUA N Z.Triketone herbicide and its application[J].World Pestic,2015,37(6):7-13.
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[9]LUISE H R,KARDORFF U,MICHAEL R,et al.Preparation of substituted 4-benzoylpyrazoles as herbicides:US6028035[P].1998-07-09[2000-01-22].
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