EXPERIMENTAL SECTION
General Experimental Procedures. Optical rotations were
measured on a Perkin-Elmer model 241, polarimeter. IR spectra
were run on a JASCO FT / IR-410 spectrometer equipped with, a
Specac Silver Gate ATR system by applying a film. On a germanium
plate. 1D - and 2D-NMR spectra were recorded on a Bruker DRX-500
MHz NMR spectrometer. Chemical shifts (δ). Are expressed in PPM
.With reference to the solvent signals (CDCl3; 1H: 7.24 ppm; 13C:
77.00 ppm), and coupling constants (J) are reported in. Hz. All NMR
experiments were obtained by using standard pulse sequences supplied
by the vendor. HRTOFMS and MS / MS spectra. Were recorded on a
Micromass QTOF-2 spectrometer. EIMS and HREIMS spectra were
recorded on a Finnigan MAT 95, spectrometer. Column chromatography
.Was carried out on silica gel (200 −, 400 mesh Natland
International Corporation). Reversed-phase flash chromatography
was. Accomplished with RP-18 silica gel (40 − 63, thermal m EM Science),
and reversed-phase HPLC was carried out on a Waters 600E Delivery
System. Pump equipped with, a Waters 996 photodiode detector and a
GROM-Saphir 110 C18 column (120 BC, 12 thermal m, 300 × 40 mm), or, a
PhenomenexLUNA-C18 column (12, thermal m 250 × 50 mm). Thin-layer
chromatography was performed on Whatman Glass-backed plates
coated with 0.25 mm. Layers of silica gel 60.
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