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This work was presented in part at the following meetings, (a) The 76th National Meeting of the Chemical Society of Japan, Yokohama, Japan, March 1999; paper 2H105.
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Special Postdoctoral Researcher under the Basic Science Program of RIKEN.
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Special Postdoctoral Researcher under the Basic Science Program of RIKEN.
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33745527842
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note
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The catalytic activity was strongly dependent on the [MMAO]/ [1] ratio. The polymerization did not occur at the ratio of [MMAO]/[1] < 50. When more than 500 equiv of MMAO was used, the catalytic activity decreased compared to that in the case of [MMAOM1] = 200. The use of PMAO (ordinary methylaluminoxane) instead of MMAO gave a polymer with lower 1,4-cis content under the same conditions.
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33745544049
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note
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The microstructure of the poly(BD) products was measured by JH NMR and 13C NMR spectroscopy (JNM EX-300) in CDC13. 'H NMR: O4.8-5.2 (=CH2 of 1,2-BD unit), 5.2-5.8 (-CH= of 1,4-BD unit and -CH= of 1,2-BD unit). 13C NMR: <5 27.4 (1,4-cis-BD unit), 32.7 (l,4-/rans-BD unit), 127.7-131.8 (1,4-BD unit), 113.8-114.8 and 143.3-144.7 (1,2-BD unit). The weight-average molecular weight (Mw), the number-average molecular weight (Mn), and the molecular weight distribution (Mw/Afn) of the polymers were measured by GPC [Shodex GPC System-11; detector, RI (RI71); column, GPC KF-508L x 2; temperature, 40 °C; eluent, THF; polystyrene standard].
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25
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33746295241
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note
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It has been well-known that the reaction of group 4 metallocene chlorides with MAO generates the corresponding metallocene alkyl cations which are similarly active as those formed in the metallocene alkyl/MAO systems. For examples, see: (a) Brintzinger, H. H.; Fischer, D.; Mülhaupt, R.; Rieger, B.; Waymouth, R. M. Angew. Chem., Int. Ed. Engl. 1995, 34, 1143. (b) Bochmann, M. J. Chem. Soc., Dalton Trans. 1996, 255. (c) Cornils, B.; Herrmann, W. A. Applied Homogeneous Catalysis with Organometallic Compounds; VCH: Weinheim, 1996. The fact that the (C5Meö)2Sm(Cl)(THF)MMAO system shows no activity for the polymerization of BD might be due to the difficulty of alkylation of (CsMea SmtClXTHF) by MMAO under the present conditions.
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2642671416
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(b) Ewen, J. A.; Elder, M. J.; Jones, R. L.; Haspeslagh, L.; Atwood, J. L.; Bptt, S. G.; Robinson, K. Makromol. Chem., Macromol. Symp. 1991, 48/49, 253. (c) Chien, J. C. W.; Tsai, W. M.; Rausch, M. D. J. Am. Chem. Soc. 1991, 113, 8570. (d) Pellecchia, C.; Longo, P.; Proto, A.; Zambelli, A. Makromol. Chem., Rapid Commun. 1992, 13, 265.
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(a) Yang, X.; Stern, C. L.; Marks, T. J. Organometallics 1991, 10, 840. (b) Ewen, J. A.; Elder, M. J.; Jones, R. L.; Haspeslagh, L.; Atwood, J. L.; Bptt, S. G.; Robinson, K. Makromol. Chem., Macromol. Symp. 1991, 48/49, 253. (c) Chien, J. C. W.; Tsai, W. M.; Rausch, M. D. J. Am. Chem. Soc. 1991, 113, 8570. (d) Pellecchia, C.; Longo, P.; Proto, A.; Zambelli, A. Makromol. Chem., Rapid Commun. 1992, 13, 265.
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Yang, X.1
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Marks, T.J.3
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33745557532
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note
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It was established that none of l/Al(i-Bu)3, l/[Ph3C][B(C6F5)4], or AKi-BuMPhaCKBtCeFs).!] showed activity under the same conditions.
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