含中心功能基氮支套索冠醚化合物的合成及其钠离子络合物的晶体结构  

Synthesis of a New N-Pivot Lariat Crown Ethers Containing Central Functional Group and the Crystal Structure of Complex with Sodium Ion

作　　者：薛国平[1] 吴成泰[1] 张绍辉[1] 周宗华[2] 

机构地区：[1]武汉大学化学系,湖北武汉420072 [2]四川大学化学系,四川成都610064

出　　处：《有机化学》1994年第3期259-264,共6页Chinese Journal of Organic Chemistry

基　　金：国家自然科学基金

摘　　要：借模板法由6,9-二氧杂-3,12-二氮杂-十四烷-1,14-二醇分别与4-甲基(或氯)-2,6-二溴甲基苯甲醚在乙腈中,以无水碳酸钠为缩合剂,制得两种尚未见文献报道的含中心功能基氮支套索冠醚化合物:N,N’-二羟乙基-16-甲基-18甲氧基-6,9-二氧杂-3,12-二氮杂-二环[12.3.1]十八-1(18),14,16-三烯(4a)和N,N'-二羟乙基-16-氯-18-甲氧基-6,9-二氧杂-3,12-二氮杂-二环[12.3.1]十八-1(18),14,16-三烯(4b)的钠离子络合物3a和3b。4a和4b经元素分析、红外光谱、核磁共振谱和质谱证实其组成和结构。借四圆衍射仪测定了3b的晶体结构和分子结构。Two novel complexes of N,N'-bis(2-hydroxyethyl)-16-methyl-18-methoxyl-6,9-dioxa-3,12-diaza-bicyclo [12.3.1] octadeca-1(18),14,16-triene(4a) and N,N'-bis(2-hydroxy-ethyl)-16-chloro-18-methoxyl-6,9-dioxa-3,12-diaza-bicyclo [12.3.1] octadeca-1 (18), 14,16-triene(4b) with sodium ion were prepared by one step reaction of 6,9-dioxa-3,12-diaza-tetradeca-1,14-diol with 4-methyl (or chloro)-2,6-bis(bromomethyl)-anisole in CH3CN at reflux temperature, using anhydrous sodium carbonate as condensing agent. They were identified by elemental analysis, IR, 1H NMR and MS. The crystal structure of complex 3b has been determined with CAD4 diffractometer. The crystal data are a = 9.767(2), b= 13.943(3), c= 1.7160(4)nm, β= 84.06(2)°, space group P21 / n, Z = 4, V=2.3255(7)nm3, Dc= 1.445g/cm3, R= 0.032 for 1794 independent reflections with I≥3σ(I).

关 键 词：氮支套索冠醚 络合物 晶体结构 钠 

分 类 号：O623.423[理学—有机化学]