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1,4,7,10-四氮杂环十二院的合成研究

A New Approach to the Synthesis of 1, 4, 7, 10-Tetraazacyclododecane

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【作者】 魏俊发卓仁禧鄢国平杜波

【Author】 WEI Jun-Fa; ZHUO Ren-Xi; YAN Guo-Ping; DU Po(Department of Chemistry, Wuhan University, Wuhan, 430072)

【机构】 武汉大学化学系!武汉430072

【Abstract】 A new and simplified method for synthesis 1, 4, 7, 10-tetraazacyclododecane (cy-clen) has been proposed by two steps in this paper. The first step deals with cyclic condensa-tion of triethylenetetramine and diethyl oxalate in methanolic solution, giving the twelve-numbered cyclic oxamide, i. e., 1, 4, 7,10-tetraazacyclododecane-2, 3-dione.The pure prod-uct was obtained as a crystalline precipitate in 39% yield on addition of ethanol to the con-centrated solution of the reaction mixture. Subsequently, in the second step, the cyclic ox-amide was reduced in THF with diborane produced in situ fr6m potassium borohydride andboron trifluoride etherate and extracted by CH2Cl2 from the basic aqueous solution of the sol-vent free residue, giving cyclen in 56% yield after removing the solvent.

【基金】 国家科学技术委员会“863”计划资助;中国博士后研究基金
  • 【文献出处】 高等学校化学学报 ,CHEMICAL RESEARCH IN CHINESE UNIVERSITIES , 编辑部邮箱 ,1997年04期
  • 【分类号】O626
  • 【被引频次】13
  • 【下载频次】438
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