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Synthesis of poly(glycidol)‐block‐poly(N‐isopropylacrylamide) copolymers using new hydrophilic poly(glycidol) macroinitiator
Authors:Sebastian Mendrek  Aleksandra Mendrek  Hans‐Jürgen Adler  Wojciech Walach  Andrzej Dworak  Dirk Kuckling
Institution:1. Fachrichtung Chemie und Lebensmittelchemie, Technische Universit?t Dresden, D‐01062 Dresden, Germany;2. Center of Polymer and Carbon Materials, M. Sklodowskiej‐Curie 34, 41‐819 Zabrze, Poland
Abstract:New, water soluble poly(glycidol) (PGl) macroinitiators for atom transfer radical polymerization (ATRP) were synthesized. This new class of macroinitiators were prepared in a three‐step process. First, series of well‐defined ω‐hydroxyl functional poly(glycidol acetal)s with different molecular weights was synthesized via anionic polymerization followed by quantitative termination of anionically growing active sites. End capping was achieved by treatment of living chain ends with water. The living nature of the system and termination reaction is discussed. In the second stage, monofunctional poly(glycidol acetal)s were functionalized by esterification with 2‐chloropropionyl chloride. Finally, selective deprotection (hydrolysis) of acetal protective groups was performed. As simultaneous partial cleavage of ester bond of attached ATRP moieties was unavoidable, the final functionality of macroinitiator calculated from 1H NMR varied in the range 85–95%. The obtained (2‐chloropropionyl) poly(glycidol) macroinitiator with DP = 55 and 90% functionality was successfully used in ATRP polymerization of N‐isopropylacrylamide (NIPAAm) at room temperature in the DMF/water mixture. Linear block copolymers with relatively narrow molecular weight distribution and controlled composition were obtained and characterized with 1H NMR and SEC‐MALLS measurements. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 2488–2499, 2008
Keywords:anionic polymerization  ATRP  diblock copolymers  macroinitiator  MALDI  poly(glycidol)  polymerization of N‐isopropylacrylamide  stimuli‐sensitive polymers
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