| 稳定同位素标记15N-N,N-二甲基苯胺的合成 |
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| 引用本文： | 杨维成,齐庆瑞,刘卫霞,李美华,罗勇.稳定同位素标记15N-N,N-二甲基苯胺的合成[J].有机化学,2012,32(1):145-148. |
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| 作者姓名： | 杨维成 齐庆瑞 刘卫霞 李美华 罗勇 |
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| 作者单位： | 1. 上海化工研究院技术开发中心 上海200062
2. 新疆教育学院职业教育分院 乌鲁木齐830046 |
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| 基金项目： | 科技部转制院所专项，质检总局科技专项 |
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| 摘 要： | 以15NH4Cl为同位素标记前体,经与苯甲酰氯胺化、霍夫曼降解得到15N标记苯胺,15N标记苯胺再与对甲苯磺酸酯进行甲基化反应,合成得到一种重要的同位素标记基础试剂15N-N,N-二甲基苯胺.以消耗的15NH4Cl计,三步反应总收率大于58.3%.产品结构经红外(IR)、核磁(NMR)、高效液相(HPLC)、质谱(MS)等表征进行确定,其化学纯度大于99.0%,同位素丰度大于98.4%15N.
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| 关 键 词： | 同位素标记 合成 N N-二甲基苯胺 表征 甲基化 |
Synthesis of Isotope-Labeled 15N-N,N-Dimethylaniline |
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| Yang,Weicheng
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Qi,Qingrui
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Liu,Weixia
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Li,Meihua
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Luo,Yong.Synthesis of Isotope-Labeled 15N-N,N-Dimethylaniline[J].Chinese Journal of Organic Chemistry,2012,32(1):145-148. |
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| Authors: | Yang Weicheng Qi Qingrui Liu Weixia Li Meihua Luo Yong |
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| Institution: | Yang,Weichenga Qi,Qingruib Liu,Weixiaa Li,Meihuaa Luo,Yong,a(a Research & Development Center,Shanghai Research Institute of Chemical Industry,Shanghai 200062)(b Branch of Professional Education,Xinjiang Normal University,Urumqi 830046) |
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| Abstract: | An efficient synthesis of 15N-N,N-dimethylaniline with 15NH4Cl as the common substrate is reported.Ammoni-ation of benzoyl chloride with 15NH4Cl provided 15N-benzamide,which was converted to 15N-aniline by Hofmann degrada-tion.Methylation of 15N-aniline with methyl p-toluenesulfonate provided 15N-N,N-dimethylaniline.The overall yield of NMR,HPLC and MS to be target compound.Its chemical purity is higher than 99.0% and isotopic enrichment is higher than 98.4% 15N. |
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| Keywords: | isotope-labeled synthesis N N-dimethylaniline characterization methylation |
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