(C_5H_(11)N_2)^+和(C_7H_(12)N_2)^(2+)的NMR研究  

An NMR Studies of (C_5H_(11)N_2)^+ and (C_7H_(12)N_2)^(2+)

作　　者：喻冲[1] 李志强[1,2] 毕研刚[1] 史旭东[1] 朱琳丽[1] 夏寺丰[1] 鲁晓明[1,2] 

机构地区：[1]首都师范大学化学系,北京100048 [2]中国科学院武汉物理与数学研究所,湖北武汉430071

出　　处：《波谱学杂志》2010年第4期524-531,共8页Chinese Journal of Magnetic Resonance

基　　金：国家自然科学基金资助项目(20871085);北京市自然科学基金资助项目(2092009)

摘　　要：结合1H NMR,13C NMR谱,分别对钨、钼配合物{WO2(C10H6O2)2(C5H11N2)2[H2N(CH2)3NH2]}3(1),{(C5H11N2)2[H2N(CH2)3NH2][MoO2(C10H6O2)2]}(2),{(C7H12N2)2[MoO2(C10H8O2)2]}(3)晶体结构中小分子环进行了归属.其中,配合物1和2中(C5H11N2)+的NMR研究证实了六元环由1,3-丙二胺和乙腈化合而成,配合物3中(C7H12N2)2+的NMR谱图证实了七元环由乙二胺和乙酰丙酮化合而成,并且推导出这些亲核加成-消除反应的反应机理.配合物1~3中的小分子环的合成在其它体系中尚未见报导,而在合成它们的反应中作为新产物随主体晶体析出,并由晶体结构解析和NMR得到了证实.The structure of small molecular rings（C5H11N2）＋ and（C7H12N2）2＋ in tungstate and molybdate complexes {WO2（C10H6O2）2（C5H11N2）2[H2N（CH2）3NH2]}3（1）,{（C5H11N2）2[H2N（CH2）3NH2][MoO2（C10H6O2）2]}（2） and {（C7H12N2）2[MoO2（C10H8O2）2]}（3） were studied by 1H-and 13C-NMR.The NMR data of（C5H11N2）＋ in complexes 1 and 2 indicated the existence of two six-membered rings,which are composed of 1,3-diaminopropane and acetonitrile.The NMR spectra of（C7H12N2）2＋ in complex 3 indicated the existence of a seven-membered ring,which is composed of ethylenediamine and acetylacetone,inferring a formation mechanism of nucleophilic addition-elimination reactions.The synthesis of small molecular rings in complexes 1~3 have not been reported in other systems.In our works,these ring structures precipitated with the host-frames as new products in complexes 1~3,as confirmed by crystal structure analysis and NMR data.

关 键 词：核磁共振(NMR) 归属 (C5H11N2)+ (C7H12N2)2+ 亲核加成-消除反应 

分 类 号：O614.61[理学—无机化学]