2-氨基乙基-二(3-氨基丙基)胺的合成

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

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。

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.