1
H, 13C and 2D NMR spectra were recorded using a JEOL
JNM a-400 spectrometer (400 MHz for 1
H NMR and
100 MHz for 13C NMR). The NMR data were measured
with in C5D5N tetramethylsilane (TMS) as internal
standard. The negative-ion mode FAB-MS spectra were
recorded on a JEOL JMS-SX 102 spectrometer. Optical
rotations were determined on a Union PM-1 digital
polarimeter.
For column chromatography, silica gel G (Scharlau
GE0049, 70-230 mesh ASTM), YMC-gel ODS (50 mm,
YMC) and highly porous copolymer resin of styrene and
divinylbenzene (Mitsubishi Chem. Ind. Co. Ltd) were used.
HPLC (Waters 515 HPLC pump) was carried on a column
of ODS (150!20 mm i.d., YMC) with a Shimadzu
refractive index (RID-6A) detector.