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一种端羟基聚酰胺-胺型分子的合成
引用本文:史俊,郭肖依,王汝斌.一种端羟基聚酰胺-胺型分子的合成[J].合成化学,2017,25(2).
作者姓名:史俊  郭肖依  王汝斌
作者单位:西安石油大学 化学化工学院,陕西 西安,710065
摘    要:以二乙醇胺和丙烯酸甲酯为原料,在甲醇中经Michael加成反应合成中间体N,N-二羟乙基-3-胺基丙酸甲酯(TAD-0.5G);TAD-0.5G与乙二胺经酰胺化缩合反应合成N,N-二羟乙基-N'-乙胺-3-胺基丙酰胺(TAD-1.0G),其结构经IR,MS(ESI)和元素分析确证。并优化了TAD-1.0G的合成条件。结果表明:在最佳合成条件TAD-0.5G 0.11 mol,n(TAD-0.5G)∶n(乙二胺)=1.6∶1.0,于35℃反应24 h]下,产率91.62%。采用MS(ESI)研究了TAD-1.0G分子裂解后的主要离子碎片和裂解途径。

关 键 词:丙烯酸甲酯  N  N-二羟乙基-3-胺基丙酸甲酯  Michael加成  酰胺化缩合  合成  裂解途径

Synthesis of An End-hydroxy PAMAM Molecular
SHI Jun,GUO Xiao-yi,WANG Ru-bin.Synthesis of An End-hydroxy PAMAM Molecular[J].Chinese Journal of Synthetic Chemistry,2017,25(2).
Authors:SHI Jun  GUO Xiao-yi  WANG Ru-bin
Abstract:The intermediate N,N-dihydroxyethyl-3-aminomethyl propanoate( TAD-0. 5G) was synthe-sized by Michael addition in MeOH, using diethanolamine and methyl acrylate as raw materials. N,N-dihydroxyethyl amine-3-aminomethyl-N′-propionamide(TAD-1. 0G) was synthesized by amide-conden-sation reaction of TAD-0. 5G with ethylenediamine. The structure was characterized by IR, MS( ESI) and elemental analysis. Then the reaction conditions were optimized. The results showed that under the optimum synthesis conditions TAD-0. 5G 0. 11 mol, n ( TAD-0. 5G ) : n ( ethylenediamine ) =1. 6 :1. 0, reaction at 35 ℃ for 24 h], the yield of TAD-1. 0 was 91. 62%. The main fragment ions and fragmentation pathway were investigated by MS( ESI) .
Keywords:methyl acrylate  N  N-dihydroxyethyl-3-aminomethyl propanoate  Michael addition  am-ide-condensation reaction  fragmentation pathway
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