Jasinski Nils, Lauer Andrea, Stals Patrick J M, Behrens Silke, Essig Sarah, Walther Andreas, Goldmann Anja S, Barner-Kowollik Christopher
Preparative Macromolecular Chemistry, Institut für Technische Chemie und Polymerchemie, Karlsruhe Institute of Technology (KIT), Engesserstr. 18, 76128 Karlsruhe, Germany.
Institut für Biologische Grenzflächen (IBG), Karlsruhe Institute of Technology (KIT), Herrmann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany.
ACS Macro Lett. 2015 Mar 17;4(3):298-301. doi: 10.1021/acsmacrolett.5b00046. Epub 2015 Feb 17.
We introduce a novel electrochemical method for the purification of complex water-soluble functional polymers contaminated with copper salts originating from copper-catalyzed azide/alkyne ligation chemistry, for which no standard purification protocol is suitable. A triethylene glycol methyl ether methacrylate (TEGMA) star polymer with 2-ureido-4-pyrimidone (UPy) end groups was prepared via an activator generated by electron transfer atom transfer radical polymerization (AGET ATRP) and copper-catalyzed azide/alkyne cycloaddition (CuAAc) and selected as a model system for electrolysis of an aqueous polymer solution. We systematically investigate the influence of sample concentration, voltage, and time of electrolysis on the quality of the purification. Atom emission spectroscopy (AES) reveals almost quantitative removal of copper, and size exclusion chromatography (SEC) as well as proton nuclear magnetic resonance spectroscopy (H NMR) ensure the full integrity of the polymer under all selected conditions.
我们介绍了一种新颖的电化学方法，用于纯化被源自铜催化的叠氮化物/炔烃连接化学的铜盐污染的复杂水溶性功能聚合物，对此没有合适的标准纯化方案。通过电子转移原子转移自由基聚合（AGET ATRP）和铜催化的叠氮化物/炔烃环加成（CuAAc）制备了具有2-脲基-4-嘧啶酮（UPy）端基的三甘醇甲基醚甲基丙烯酸酯（TEGMA）星形聚合物，并将其选作聚合物水溶液电解的模型体系。我们系统地研究了样品浓度、电压和电解时间对纯化质量的影响。原子发射光谱（AES）显示几乎能定量去除铜，尺寸排阻色谱（SEC）以及质子核磁共振光谱（H NMR）确保了在所有选定条件下聚合物的完整性。
