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Ga(OTf)3催化合成苯并二氮杂卓及其结构解析
引用本文:王璐,潘向强,蔡晶晶,邹建平.Ga(OTf)3催化合成苯并二氮杂卓及其结构解析[J].波谱学杂志,2011,28(3):383-389.
作者姓名:王璐  潘向强  蔡晶晶  邹建平
作者单位:苏州大学分析测试中心,江苏苏州,215123;苏州大学材料与化学化工学部,江苏省有机合成重点实验室,江苏苏州215123
基金项目:国家自然科学基金资助项目(20772088)
摘    要:以邻苯二胺和丙炔酸酯为原料,Ga(OTf)3催化一锅法合成了一类新型的1,5-苯并二氮杂卓衍生物,超声波辅助加快了反应的进行,该反应条件温和,反应时间短. 利用1H NMR、13C NMR 确定了该产物的结构,并通过DEPT、1H-1H COSY、HMQC、HMBC等2D NMR谱,对化合物的1H NMR和13C NMR数据进行了详细的归属,讨论了化合物的质谱裂解规律,进一步确证了该化合物的结构.

关 键 词:核磁共振(NMR)  归属  2D  NMR  飞行时间质谱  1  5-苯并二氮杂卓  Ga(OTf)3
收稿时间:2010-12-07

Synthesis and Spectroscopic Characterization of a Novel 1,5-Dibenzodiazepine Derivative
WANG Lu,PAN Xiang-qiang,CAI Jing-jing,ZOU Jian-ping.Synthesis and Spectroscopic Characterization of a Novel 1,5-Dibenzodiazepine Derivative[J].Chinese Journal of Magnetic Resonance,2011,28(3):383-389.
Authors:WANG Lu  PAN Xiang-qiang  CAI Jing-jing  ZOU Jian-ping
Institution:1. Testing and Analysis Center, Soochow University, Suzhou 215123, China;; 2. Key Laboratory of Organic Synthesis of Jiangsu Province, College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou 215123, China
Abstract:Gallium (III) triflate-catalyzed reaction between o-phenylenediamine and ethyl propiolate under solvent-free and ultrasonic irradiation conditions produced a novel 1, 5-benzodiazepine derivative with a yield rate of 88%. Complete assignment of the 1H and 13C NMR chemical shift of the compound was obtained using 2D NMR techniques, including DEPT, 1H-1H COSY, 1H-13C HMQC and 1H-13C HMBC. Mass fragmentation pathway was proposed based on the high resolution MS spectrum of the compound.
Keywords:NMR  assignment  2D NMR  TOF MS  1  5-benzodiazepine derivative  Ga(OTf)3  
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