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note
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-1; T = 296 K; R1 = 0.059 for 4577 observations, space group P-1(#2). Crystallographic data (excluding structure factors) for the structure in this paper have been deposited with the Cambridge Crystallographic Data Centre as a supplementary number CCDC 277890. Copies of the data can be obtained, free of charge, on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK [fax: +44(0) 1223 336033 or e-mail: deposit@ccdc.cam.ac.uk].
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24
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33645337141
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note
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3 (30 mL × 3). The organic layer was dried over anhydrous sodium sulfate and evaporated to give an oily residue, which was purified by silica gel column chromatography (n-hexane to AcOEt/n-hexane = 1/20) to give pure 6a (50 mg, 79%) as a colorless solid. Analytical sample was obtained by recrystallization from AcOEt (mp 224°C).
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25
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13C NMR signals because of their broadening.
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