蒽加氢产物的结构指认和定量核磁共振分析  

Structural Elucidation and Quantitative Analysis of Hydrogenation Products of Anthracene by NMR Spectroscopy

作　　者：窦梦雨 赵奇 侯相林[1,2] 刘雷 唐明兴[1] 王英雄[1,2] DOU Meng-yu;ZHAO Qi;HOU Xiang-lin;LIU Lei;TANG Ming-xing;WANG Ying-xiong(Institute of Coal Chemistry,Chinese Academy of Sciences,Taiyuan 030001,China;Center of Materials Science and Optoelectronics Engineering,University of Chinese Academy of Sciences,Beijing 100049,China;School of Chemistry and Chemical Engineering,Taiyuan University of Technology,Taiyuan 030024,China)

机构地区：[1]中国科学院山西煤炭化学研究所,山西太原030001 [2]中国科学院大学,材料与光电研究中心,北京100049 [3]太原理工大学化学化工学院,山西太原030024

出　　处：《波谱学杂志》2021年第2期239-248,共10页Chinese Journal of Magnetic Resonance

基　　金：国家自然科学基金山西低碳联合基金重点支持项目(U1910202).

摘　　要：本文利用多种液体核磁共振(NMR)技术,综合分析了在三个不同反应条件下蒽催化加氢反应获得的产物混合物.利用二维扩散排序谱(DOSY)和一维选择性激发谱(selTOCSY)确定了产物中含有的二氢蒽、四氢蒽、对称八氢蒽和非对称八氢蒽;利用^(1)H NMR、^(13)C NMR、DEPT135、^(1)H-^(1)H COSY、^(1)H-^(13)C HSQC实验对二氢蒽、四氢蒽和对称八氢蒽的^(1)H和^(13)CNMR信号进行了详细归属;利用定量核磁共振氢谱(QNMR)计算得到了蒽的转化率和产物的选择性.本研究可用于指导优化催化反应条件,提高产物对称八氢蒽的选择性,同时为稠环类芳烃催化加氢产物的分析提供系统的NMR技术方案.Three product mixtures of anthracene catalytic hydrogenation under different catalytic conditions were analyzed by nuclear magnetic resonance(NMR)spectroscopy.Dihydroanthracene,tetrahydroanthracene,symmetric octahydroanthracene,and asymmetric octahydroanthracene were successfully detected with diffusion-ordered spectroscopy(DOSY)and one-dimension selective gradient total correlation spectroscopy(selTOCSY)techniques.The^(1)H and^(13)C NMR signals of dihydroanthracene,tetrahydroanthracene and symmetric octahydroanthracene were assigned by^(1)H NMR,^(13)C NMR,DEPT135,^(1)H-^(1)H COSY,^(1)H-^(13)C HSQC.The conversion of anthracene and selectivity of the products were calculated by quantitative^(1)H NMR(QNMR).The results demonstrated that NMR is a versatile and powerful tool to guide and optimize catalytic reaction conditions for increasing the selectivity of symmetrical octahydroanthracene.The present research provides a systematic NMR analysis scheme for polycyclic aromatic hydrocarbons catalytic hydrogenation.

关 键 词：液体核磁共振 结构指认 二维扩散排序谱(DOSY) 一维选择性激发谱(selTOCSY) 定量核磁共振氢谱(QNMR) 蒽催化加氢 

分 类 号：O482.53[理学—固体物理]