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Crosslinking and ageing of C labelled polyisoprene part 1: Synthesis and polymerisation of 4-C-isoprene |
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| Authors: | Jean-François Pilichowski Myriam Morel Farba Tamboura Stefan Chmela Jacques Lacoste |
| Institution: | a Clermont Université, Université Blaise Pascal, Laboratoire de Photochimie Moléculaire et Macromoléculaire, BP 10448, F-63000 Clermont-Ferrand, France b CNRS, UMR 6505, LPMM, F-63177 Aubiere cedex, France c Polymer Institute, Slovak Academy of Sciences, Dubravka Cesta 9, 842 34 Bratislava, Slovak Republic d Clermont Université, ENSCCF, Laboratoire de Photochimie Moléculaire et Macromoléculaire, BP 10448, F-63000 Clermont-Ferrand, France |
| Abstract: | 4-13C-isoprene was prepared by the Wittig reaction. All reaction steps were optimised using unlabelled compounds. By reaction with triphenyl phosphine, 13C labelled methyl iodide afforded labelled methyl-triphenyl phosphine iodide in 84% yield. This reacted with meth acrolein with production of 4-13C-isoprene in 64% yield. Labelled polyisoprene was prepared by anionic polymerisation initiated by t-butyl lithium. Based on 13CH3I the overall yield is ca 30%. The polymer was characterized by 1H and 13C NMR spectroscopy. The contribution of each microstructure was cis 1-4, 72%]; trans 1-4, 10%]; 3-4, 18%]. |
| Keywords: | 4-13C-Isoprene 13C-polyisoprene NMR Elastomer degradation |
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