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34548751759
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Characterization of 1 Mp 198°C. 1H NMR (400 MHz, CDCl3, δ, 7.58 (d, 3J, 8.5 Hz, 4 H, Har, 7.53 (d, 3J, 8.5 Hz, 4 H, Har, 7.49 (d, 3J, 8.8 Hz, 4 H, Har, 7.15 (s, 2 H, Har, 6.92 (d, 3J, 8.8 Hz, 4 H, Har, 5.86 (ddt, 3Jtrans, 17.0 Hz, 3Jcis, 10.4 Hz, 3J, 6.7 Hz, 2 H, HC, 5.12 (dm, 3Jtrans, 17.0 Hz, 2 H, CHtrans, 5.05 (dm, 3Jcis, 10.4 Hz, 2 H, CHcis, 4.00 (t, 3J, 6.7, 4 H, CH2, 2.51 (q, 3J, 6.7, 4 H, CH2, 1.28 (s, 9 H, t-Bu, 13C NMR (100 MHz, CDCl3, δ, 158.5 (C, 141.7 (C, 139.7 (C, 138.3 (C, 137,5 (C, 134.4 (CH, 133.2 (C, 129.8 (CH, 128.0 CH, 12
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9d structure refinement SHELXL-97 (G. M. Sheldrick, Universität Göttingen, 1997), graphics SCHAKAL (E. Keller, Universität Freiburg, 1997). CCDC 649216 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at www.ccdc.cam.ac.uk/conts/ retrieving.html [or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 (1223)336033, E-mail: deposit@ccdc.cam.ac. uk].
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0038414570
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33847029547
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Angew. Chem. 2006, 118, 3845.
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Lautens, M.1
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23
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34548782176
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Characterization of 6 Mp >250°C. 1H NMR (300 MHz, CDCl3, δ, 7.53 (d, 3J, 8.4 Hz, 8 H, Har, 7.49-7.40 (m, 16 H, Har, 7.12 (s, 4 H, H ar, 6.86 (d, 3J, 8.7 Hz, 8 H, Har, 3.98 (t, 3J, 6.2 Hz, 8 H, CH2, 1.82 (m, 8 H, CH2, 1.53 (m, 8 H, CH2, 1.26 (s, 18 H, t-Bu, 13C NMR (75 MHz, CDCl3, δ, 158.7 (C, 141.0 (C, 139.6 (C, 138.5 (C, 138.4 (C, 133.1 (C, 129.8 (CH, 128.0 (CH, 127.3 (C, 127.0 (CH, 126.6 (CH, 115.0 (CH, 67.5 (CH2, 34.1 (C, 31.6 (CH3, 28.6 (CH2, 25.0 CH2, ESI-MS, m/z, 1135.4 [MH, C80H82N 2O4, H, Anal. Calcd for C80H 82N2O4·H2O: C, 83.30; H, 7.34; N, 2.43. Found: C
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2O: C, 83.30; H, 7.34; N, 2.43. Found: C, 83.47; H, 7.37; N, 1.99.
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