spectra were obtained using a Shimadzu UV-2401 PC spectrophotometer. IR spectra
were recorded on a Bruker Tensor-27 infrared spectrophotometer using KBr pellets.
1D and 2D NMR spectra were performed on Bruker AM-400 and DRX-500 spectrometers
(Bruker BioSpin GmBH, Rheinstetten, Germany) with TMS as the internal standard.
ESIMS spectra were recorded on a Bruker HTC/Esquire spectrometer. HREIMS was
recorded on a Waters AutoSpec Premier P776 spectrometer. Column Chromatography
(CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Ltd.,
Qingdao, China), Rp-18 (40–63 μm, Merk). Fractions were monitored by TLC (GF254,
Qingdao Marine Chemical Ltd., Qingdao, China), and by heating silica gel plates
sprayed with 10% H2SO4 in ethanol.
GC analysis was performed on an HP5890 gas chromatograph equipped with a
H2 flame ionization detector.