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0345559989
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note
-
Initial experiments indicated that the low solubility of 13 in the aqueous reaction medium posed difficulties in accurate sampling for analysis by chiral-phase HPLC. On the other hand, complete extractions of reaction mixtures provided >90% mass recovery. Parallel reactions were therefore started simultaneously, and then each reaction mixture was extracted completely after a given period of time. All samples were analyzed by chiral-phase HPLC, which cleanly resolved 13 and the four possible reduced products.
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0345128442
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note
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Details of this crystal structure will be published elsewhere.
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63
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20644469267
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0345559988
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note
-
Analytical samples were prepared by vortexing 0.5 mL of the reaction mixture with 0.5 mL of EtOAc. After the mixture was centrifuged at 7500 rpm for 1 min, the organic layer was removed, filtered, and analyzed by HPLC.
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