Xia Dao-hong
2009
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Journal
Fine chemicals
Abstract
2-aminoethyl-bis(3-aminopropyl)amine was synthesized with bulk chemicals.N-Acetylethylenediamine was first prepared through the reaction between ethylenediamine and ethyl acetate.The optimal reaction condition is n(ethylenediamine)/n(ethyl acetate)=4 with refluxing for 24 h.The yield is 80.8 %.Then,N-Acetylethylenediamine reacted with 2 equivalents of acrylonitrile activated by a little water at 70 ℃ to form the nitrile intermediate.Finally,Hydrazine reduced the nitrile group of the intermediate catalyzed by Raney Ni,and then the acetyl group was hydrolyzed to give 2-aminoethyl-bis(3-aminopropyl)amine with the overall isolated yield 60%.Every step was detected with TLC.The intermediates and the objective compound were characterized with 1HNMR and elemental analysis.