节点文献
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
【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.
【Key words】 Synthesis; Polyazacycloalkyl compound; 1; 4; 7; 10-Tetraazacyclododecane; Cyclic condensation;
- 【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