4,7,10-三(叔丁氧碳酰甲基)-1,4,7,10-四氮杂环十二烷-1-乙酰肼的微波合成  

Microwave Synthesis of 4,7,10-Tris(tert-butoxycarbonylmethyl)-1,4,7,10-tetraazacyclodo-decane-1-acetohydrazide

作　　者：周进 杨海东 孙宏顺 李玉龙 蒋蕻 ZHOU Jin YANG Hai-dong SUN Hong-shun LI Yu-long JIANG Hong(Targeted MRI Contrast Agents Laboratory of Jiangsu Province, Nanjing Polytechnic Institute, Nanjing 210048, 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

出　　处：《合成化学》2017年第2期159-162,共4页Chinese Journal of Synthetic Chemistry

基　　金：江苏省高等学校大学生创新创业训练计划项目(201512920027H);江苏高校品牌专业建设工程资助项目;南京科技职业学院院级重点项目(NHKY-2015-1)

摘　　要：以轮环藤宁为起始原料,依次与溴乙酸叔丁酯,溴乙酸乙酯和水合肼反应合成了一种核磁共振对比剂螯合前体——4,7-10-三(叔丁氧碳酰甲基)-1,4,7,10-四氮杂环十二烷-1-乙酰肼(4),其结构经~1H NMR,^(13)C NMR,FT-IR和MS(ESI)表征。研究了溶剂、水合肼用量、微波功率和反应时间对4收率的影响。结果表明:乙醇为溶剂,水合肼10 eq.,于400 W微波反应10 min,4(粉末固体)收率90%。A chelator precursor for MRI contrast agent, 4,7,10-tris （tert-butoxycarbonylmethyl） -1,4, 7,10-tetraazacyclodo-decane-l-acetohydrazide（4）, was synthesized using cyclen as the starting materi- al, then reaction with tert-butyl bromoacetate, ethyl bromoacetate and hydrazine hydrate, respectively. The structure was characterized by 1H NMR, 13C NMR, FT-IR and MS （ESI）. The effects of solvents, molar ratio of hydrazine hydrate, microwave power and reaction time on the yield of 4 were investigated. The optimum conditions were as follows： ethanol as solvent, hydrazine hydrate 10 eq. , microwave irradiation for 10min under 400 W, the yield of 4（powder solid） was 90%.

关 键 词：轮环藤宁 核磁共振对比剂 螯合前体 微波合成 

分 类 号：O623.7[理学—有机化学]