| 稳定同位素标记[2H4]-β-紫罗兰酮的合成及表征 |
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| 引用本文： | 白冰,钟闻英,黄备备,张改红,贾春晓,毛多斌.稳定同位素标记[2H4]-β-紫罗兰酮的合成及表征[J].化学试剂,2020,42(3):332-336. |
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| 作者姓名： | 白冰 钟闻英 黄备备 张改红 贾春晓 毛多斌 |
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| 作者单位： | 郑州轻工业大学食品与生物工程学院,河南郑州450000;郑州轻工业大学材料与化学工程学院,河南郑州450000 |
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| 基金项目： | 河南省科技攻关计划;烟草行业烟草工业生物技术重点实验室专项项目;国家自然科学基金 |
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| 摘 要： | 以柠檬醛为原料,以D6-丙酮为稳定同位素标记前体物,经碱催化羟醛缩合及酸催化关环反应合成了2H4]-β-紫罗兰酮,考察了碱和酸的种类、用量及温度对反应的影响,确定了最优路线:先在20%NaOH重水溶液中于55℃反应2 h合成假性紫罗兰酮,再经浓硫酸于-10℃反应10 min合成目标产物,两步总收率为60%。目标化合物结构通过质谱、核磁共振氢谱、核磁共振碳谱、红外光谱进行表征,经高效液相色谱确认化学纯度>99%,经计算同位素丰度为98.1%。该方法所得目标产物可作为稳定同位素稀释分析法中的对照物质。
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| 关 键 词： | 同位素标记 合成 [2H4]-β-紫罗兰酮 柠檬醛 对照品 |
Synthesis and Characterization of Stabilized Isotope [2H4]-β-Ionone |
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| BAI Bing,ZHONG Wen-ying,HAUNG Bei-bei,ZHANG Gai-hong,JIA Chun-xiao,MAO Duo-bin.Synthesis and Characterization of Stabilized Isotope [2H4]-β-Ionone[J].Chemical Reagents,2020,42(3):332-336. |
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| Authors: | BAI Bing ZHONG Wen-ying HAUNG Bei-bei ZHANG Gai-hong JIA Chun-xiao MAO Duo-bin |
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| Affiliation: | (School of Food&Biological Engineering,Zhengzhou University of Light Industry,Zhengzhou 450000,China;College of Material and Chem ical Engineering,Zhengzhou University of Light Industry,Zhengzhou 450000,China) |
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| Abstract: | Stabilized isotope-labeled 2H4]-β-ionone was synthesized by using citral as starting material and D6-acetone as a stable isotope-labeled precursor with two steps.The optimal reaction conditions were investigated.The first step was aldol condensation of citral with D6-acetone in the presence of 20% NaOH at 55 ℃ for 2 h.The second step was cyclization of the acquired pseudoionone in the presence of concentrated H2SO4 at-10 ℃ for 10 min.The total yield was 60%.The target compound was confirmed by MS,1HNMR,13CNMR and IR.The chemical purity was 99% detected by HPLC,and the isotope abundance was 98.1% by calculation.The compound could be used as standard in the method of stable isotope dilution. |
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| Keywords: | isotope labeled synthesis [2H4]-β-ionone citral reference substance |
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