連続フロー法核磁気共鳴装置の開発と分子ダイナミックスへの利用

连续流核磁共振仪的研制及其在分子动力学中的应用

• 批准号: 07650976
• 负责人: KOSUGI Yoshio
• 金额: $ 1.15万
• 依托单位: SHIMANE UNIVERSITY (1996)Nagoya University (1995)
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 1995
• 资助国家: 日本
• 起止时间: 1995 至 1996
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-07650976/
• 关键词: NMR; MOLECULAR DYNAMICS; DIBENZOPHENAZINE; ASCORBIC ACID; MR CONTRAST AGENT; NMR DATA COLLECTION; CARBON DIOXIDE; KOLBE-SCHMITT REACTION; 分子ダイナミックス; MRI造影剤; ジヒドロナフトフランジオール; タ-フェニル型複素環化合物; 重水素化アスコルビン酸; MRI用造影剤

A simple flow system in combination with liquid-chromatography has been developed, and NMR data compiled in the personal computer have been useful for analyzing new complex spectra. Thus various research projects have been accomplished using a dynamic method.1) A new reaction of 1-naphthyliminodimagnesium dibromide to give dibenzo-phenazine was clarified y the NMR identification of four isomers. Based on the result obtained, the known Ullmann-Ankersmit reaction has been corrected, and a selective preparation of the [a.j] isomer has been found.2) The protective action of ascorbic acid against radicals caused by gamma-ray has been investigated in the relation with DNA mutation. The dynamics have also been applied to new developements of MR contrast agent.3) The present method has been effectively used for the analysis of complex spectra of furan derivatives for new polymer and, of terphenyl heterocyclics for electroluminescence elements.4) The transferring to Shimane University in Heisei 8th year forced us to change a part of experimental methods, since no liquid chromatography was available for use. One of new projects was the study on the [phenolate・CO2] complex in the Kolbe-Schmitt reaction unsolved for long time. The dynamic NMR has proved the complex without any doubt, and determined the structure.

一个简单的流动系统与液相色谱相结合，已被开发，并在个人计算机上编译的NMR数据已被用于分析新的复杂的光谱。1）通过对四种异构体的NMR鉴定，阐明了1-萘亚氨基二溴化二镁生成二苯并吩嗪的新反应。在此基础上，对已知的Ullmann-Ankersmit反应进行了修正，并找到了[a，j]异构体的选择性制备方法。2）研究了抗坏血酸对γ射线引起的自由基的保护作用与DNA突变的关系。该动力学也被应用于MR造影剂的新开发。3）本方法已有效地用于分析新聚合物的呋喃衍生物和电致发光元件的三联苯杂环化合物的复杂光谱。4）转移到平成岛根大学第8年迫使我们改变了一部分实验方法，因为没有液相色谱可供使用。新的研究课题之一是对Kolbe-Schmitt反应中长期未解决的[酚盐·CO2]络合物的研究。动态核磁共振谱证实了配合物的存在，并确定了配合物的结构。

项目成果

. Kosugi: "Unexpected Formation of Dibenzophenazines." J. Org. Chem. 60(17). 5690-5692 (1995)

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M. Suzuki: "Magnetic Characterization of Magnetite Particles for MR contrst Agents" Bull. Chem : Soc. Jpn.69(4). 1143-1148 (1996)

M. Suzuki：“MR 对比剂的磁铁矿颗粒的磁性表征”公牛。

Y.Kosugi: "Is It the Same or a Different Product in Ullman-Ankersmit and Horner-Dehnert Reactions?" J.Chemical Research. M.(1). M0185-0197 (1995)

Y.Kosugi：“Ullman-Ankersmit 和 Horner-Dehnert 反应中的产物是相同还是不同？”