含N、O配体的合成及其相关配合物的表征分析  

Synthesis of N,O Ligands and the Structure Characterization of its Complex

作　　者：王莹莹[1] 王秋月[1] 刘为铸 花尔并[1] 

机构地区：[1]天津科技大学生物工程学院,天津300457

出　　处：《天津科技大学学报》2014年第1期20-24,共5页Journal of Tianjin University of Science & Technology

基　　金：国家自然科学基金资助项目(81072521);天津科技大学人才引进科研启动基金资助项目(20091204)

摘　　要：根据桥联配体的特性,通过中间体二(2–吡啶甲基)胺(DPA)的合成,设计并合成3个含N、O的配体,分别是:三(2–吡啶甲基)胺(TPA)、二(2–吡啶甲基)(6–氯甲基–2–吡啶甲基)胺(TPA-Cl)、N–苯甲酰–2–甲苯羟胺(BOTHAH).合成DPA和TPA时,采用醛胺缩合形成席夫碱并进行还原,即"一锅法".再以2,6–吡啶二甲酸为原料通过酯化、还原、氯变、取代反应合成2,6–二氯甲基吡啶,与DPA反应生成TPA的衍生物.同时,以2–硝基甲苯为原料,通过锌粉还原生成2–甲苯羟胺,2–甲苯羟胺与苯甲酰氯发生酰化反应,合成异羟肟酸型的N、O配体BOTHAH.并用1H,NMR分别对DPA、TPA、TPA-Cl、BOTHAH配体进行结构表征分析,采用红外吸收光谱表征相关过渡金属配合物的结构.According to the characteristics of bridging ligands,three ligands were synthesized,which are 1-（pyridine-2-yl）-N ,N-bis（pyridine-2-ylmethyl）methanamine（TPA）,[6-（chloromethyl）pyridine-2-yl]-N ,N-bis（pyridine-2-ylmethyl）metha-namine（TPA-Cl）and N-benzoyl-o-tolyl hydroxylamine（BOTHAH）,including one intermediate,bis（pyridine-2-ylmethyl） amine（DPA）. Bis（pyridine-2-ylmethyl）amine（DPA）and TPA were synthesized with “one-pot reaction” through amine-aldehyde condensation to form the Schiff base first and then followed by reduction. The new TPA derivatives are based on DPA and pyridine,2,6-（dichloromethyl）which is synthetized from 2,6-Pyridinedicarboxylic acid by esterification, reduction and substitution reactions. In addition,BOTHAH,another hydroxamic acid ligand of N,O elements,was also synthetized. The structures of the compounds were characterized with1H NMR and the structures of the coordination com-plex were analysed with IR.

关 键 词：O配体 合成 铁 锰配合物 

分 类 号：O621.3[理学—有机化学]