2-氨基乙基-二(3-氨基丙基)胺的合成

该文用大宗化工原料合成了2-氨基乙基-二(3-氨基丙基)胺。首先,乙二胺与乙酸乙酯反应生成N-乙酰基乙二胺,最佳反应条件为:n(乙二胺)/n(乙酸乙酯)=4,回流反应24 h,收率80.8%;然后在70℃,少量水作用下,N-乙酰基乙二胺与两分子丙烯腈加成;最后Raney Ni催化水合肼还原腈基,水解脱酰基,得到2-氨基乙基-二(3-氨基丙基)胺。TLC检测每一步反应,综合收率60%。对中间体和目标产物进行了核磁共振和元素分析表征。

Synthesis of 2-Aminoethyl-bis(3-aminopropyl)amine

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.