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采用3种合成策略来制备(苯胺齐聚物-b-聚乙二醇)3三臂星型刚柔嵌段共聚物,获得了预期的目标产物.对每一种合成策略中各阶段的产物进行了结构表征,分析讨论了氧化偶联策略A和“先臂后核”缩合策略B的优点以及存在的问题,最终发展了简单、高效的“先核后臂”缩合策略C,即从均苯三甲酰氯和氨基/羧基封端苯胺四聚体出发,通过酰基化反应得到单分散的苯胺四聚体星型中间体M03,然后以1-乙基-(3-二甲基氨基丙基)碳酰二亚胺盐酸盐(EDCI)和4-二甲氨基吡啶(DMAP)为催化剂,使星型中间体M03与聚乙二醇单甲醚(m-PEG 550)经过脱水缩合反应得到(苯胺四聚体-b-聚乙二醇)3星型刚柔嵌段共聚物,并用红外光谱、质谱、核磁氢谱等进行了表征,表明所获得的产物与预期结构一致.
Three kinds of synthesis strategies were used to prepare the three-arm star-shaped rigid-rigid block copolymers (aniline oligomer-b-polyethylene glycol) 3, and the expected target products were obtained.For each of the synthetic strategies, The structure and characteristics of oxidative coupling strategy A and the strategy of “forearm posterior nucleus” and “condensation strategy B” were analyzed and discussed. Finally, a simple and efficient “pronucleus” strategy was developed. , Starting from trimesoyl chloride and amino / carboxyl terminated aniline tetramer, monodisperse aniline tetrameric star intermediate M03 was obtained by acylation reaction, and then was synthesized with 1-ethyl- (3-dimethyl Aminopropyl) carbodiimide hydrochloride (EDCI) and 4-dimethylaminopyridine (DMAP) as catalysts, star-shaped intermediate M03 and polyethylene glycol monomethyl ether (m-PEG 550) Condensation reaction to get (aniline tetramer -b-polyethylene glycol) 3-star rigid-flexible block copolymers, and characterized by IR, MS, 1H NMR spectra showed that the obtained product is consistent with the expected structure.