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48949121094
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note
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6) δ ppm 1.35 (q, J = 12.81, 12.72, 12.72 Hz, 1H), 1.53 (m, 1H), 1.76 (dd, J = 25.80, 12.78 Hz, 1H), 2.07 (s, 1H), 2.50 (s, 1H), 2.89 (d, J = 11.30 Hz, 1H), 3.02 (d, J = 13.45 Hz, 1H), 3.44 (d, J = 10.29 Hz, 1H), 3.55 (d, J = 13.55 Hz, 1H), 4.26 (s, 1H), 7.26 (m, 1H), 7.61 (d, J = 7.83 Hz, 1H), 7.81 (t, J = 7.38, 7.38 Hz, 1H), 8.51 (d, J = 4.13 Hz, 1H).
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36
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48949121093
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note
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Enantiomeric excess analysis was determined by HPLC with a Chiralcel-OD column at 254 nm (hexane/iPrOH in the ratio of 97/3, flow 0.5 mL/min; the retention time of (R)-2 was 17.6 min, while that of (S)-2 was 19.5 min).
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37
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48949121092
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note
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-3. X-ray data were collected with Bruker SMART APEX CCD diffractometer with graphite-monochromatized Mo Kα radiation (λ = 0.71073 Å) operated at 2.0 kW (50 kV, 40 mA). The structures were solved by direct methods with the program shelxs-97. All non-hydrogen atoms were refined anisotropically. The details of the crystallographic data have been deposited with Cambridge Crystallographic Data Centre as supplementary publication NO. CCDC 682454.
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43
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9444236231
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Braga, A.L.1
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