1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸三叔丁酯的合成  

Synthesis of Tri-tert-butyl 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate

作　　者：刘莎莉 李睿哲 周进 蒋蕻 李玉龙 孙宏顺 LIU Sha-li;LI Rui-zhe;ZHOU Jin;JIANG Hong;LI Yu-long;SUN Hong-shun(Targeted MRI Contrast Agents Laboratory of Jiangsu Province,Nanjing Polytechnic Institute,Nanjing 210048,China;College of Chemistry and Molecular Engineering,Nanjing University of Technology,Nanjing 211816,China)

机构地区：[1]南京科技职业学院,江苏省磁共振靶向显像剂工程实验室,江苏南京210048 [2]南京工业大学化学与分子工程学院,江苏南京211816

出　　处：《安徽化工》2021年第3期27-30,共4页Anhui Chemical Industry

基　　金：江苏省高等学校大学生创新创业训练计划项目(编号:202012920001Y);江苏省自然科学基金(编号:BK20181486);江苏省高校自然科学基金(编号:17KJB320001);江苏省高校优秀中青年教师和校长境外研修计划;江苏省青蓝工程资助项目。

摘　　要：以轮环藤宁和溴乙酸叔丁酯为原料,制得中间体1,4,7,10-四氮杂环十二烷-1,4,7-三乙酸叔丁酯溴酸盐(2),然后利用中间体2设计了两条合成路线:第一条合成路线为与溴乙酸反应直接得到产物;第二条合成路线为先与溴乙酸乙酯反应,再水解得到产物,最终目标产物为1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸三叔丁酯(4),并对反应条件进行了优化。产物结构经1H NMR、13C NMR、IR和MS(ESI)确证。Intermediate 1,4,7-tris(tert-butoxycarbonylmethyl)-1,4,7,10-tetraazacyclododecane hydrobro-mide(2)was obtained from cyclen and tert-butyl bromoacetate.Then two different routines were designed and successfully got the final product tri-tert-butyl 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate(4).One synthetic route was that intermedi⁃ate 2 react directly with bromoacetic acid,another route was that intermediate 2 react with ethyl bromoacetate then hydro⁃lyzed.The structure was confirmed by1H NMR,13C NMR,FT-IR and MS(ESI).

关 键 词：轮环藤宁 对比剂 合成 磁共振成像 

分 类 号：O623.7[理学—有机化学]