NMR analysis was performed on a Varian Inova 600-MHz spectrometer. The sample was deuterium-exchanged by lyophilization from D2O and dissolved in 0.5 mL D2O. The 1H-NMR 1-D and 2-D TOCSY (total correlation spectroscopy) spectra were acquired at 25(C. Proton chemical shifts were measured relative to an internal acetone standard ((=2.225 ppm). 1H-NMR data were compared with those of a previous sample having the structure proposed for this sample. The data confirmed an identical structure for the major component of this sample, but also suggested the presence of a truncated component.
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