高等学校化学学报 ›› 1997, Vol. 18 ›› Issue (4): 658.

• 研究简报 • 上一篇    下一篇

1,4,7,10-四氮杂环十二院的合成研究

魏俊发, 卓仁禧, 鄢国平, 杜波   

  1. 武汉大学化学系, 武汉, 430072
  • 收稿日期:1996-04-15 出版日期:1997-05-24 发布日期:1997-05-24
  • 通讯作者: 卓仁禧.
  • 作者简介:魏俊发, 男, 33岁, 博士后.
  • 基金资助:

    国家科学技术委员会“863”计划资助;中国博士后研究基金

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

WEI Jun-Fa, ZHUO Ren-Xi, YAN Guo-Ping, DU Po   

  1. Department of Chemistry, Wuhan University, Wuhan, 430072
  • Received:1996-04-15 Online:1997-05-24 Published:1997-05-24

关键词: 合成, 多氮杂环烷烃, 1, 4, 7, 10-四氮杂环十二烷, 环化缩合

Abstract: Anew 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 THFwith 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.

Key words: Synthesis, Polyazacycloalkyl compound, 1,4,7,10-Tetraazacyclododecane, Cyclic condensation

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