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

摘要

A chelator precursor for MRI contrast agent, 4,7,10-tris( tert-butoxycarbonylmethyl)-1,4, 7,10-tetraazacyclodo-decane-1-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 1 H NMR, 13 C 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 investiga-ted. The optimum conditions were as follows:ethanol as solvent, hydrazine hydrate 10 eq. , microwave irradiation for 10 min under 400 W, the yield of 4(powder solid) was 90%.%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,13C 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%.