C 605

Optical rotations were measured on a Jasco P-1020 automatic digital polarimeter. UV spectra were obtained in an HPLC (Agilent 1200, DAD). IR spectra were obtained using a Bruker Tensor 27 FT-IR spectrometer with KBr pellets. NMR spectra were acquired with a Bruker Avance III 600 instrument at room temperature. EIMS (including HREIMS) was measured on a Waters AutoSpec Premier P776 spectrometer. Silica gel (200–300 mesh, Qingdao Marine Chemical, Inc., Qingdao, P. R. China), MCI CHP-20 (70–150 μm, Mitsubishi Chemical Corporation, Japan) and Sephadex LH-20 (Amersham Biosciences, Sweden) were used for column chromatography (CC). Medium pressure liquid chromatography (MPLC) was performed on a Büchi Sepacore System equipping with pump manager C-615, pump modules C-605, and fraction collector C-660 (Büchi Labor technik AG, Switzerland), and columns packed with Chromatorex C-18 (40–75 μm, Fuji Silysia Chemical Ltd., Japan). Fractions were monitored by TLC and HPLC (Agilent 1200, Extend-C18 column, 5 μm, 4.6 × 150 mm).

Melting points were obtained on an X-4 micro melting point apparatus. Optical rotations were measured with a Horiba SEPA-300 polarimeter. IR spectra were obtained with a Tenor 27 spectrophotometer using KBr pellets. 1D and 2D spectra were run on a Bruker Avance III 600 MHz spectrometer with TMS as an internal standard. Chemical shifts (δ) were expressed in ppm with reference to the solvent signals. Mass spectra were recorded on an Agilent 6200 Q-TOF MS system. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, People’s Republic of China), RP-18 gel (20–45 µm, Fuji Silysia Chemical Ltd., Japan), and Sephadex LH-20 (Pharmacia Fine Chemical Co., Ltd., Sweden). Medium Pressure Liquid Chromatography (MPLC) was performed on a Büchi Sepacore System equipping with pump manager C-615, pump modules C-605 and fraction collector C-660 (Büchi Labortechnik AG, Flawil, Switzerland), and columns packed with RP-18 gel. Preparative High Performance Liquid Chromatography (prep-HPLC) was performed on an Agilent 1260 liquid chromatography system equipped with Zorbax SB-C18 columns (5 μm, 9.4 mm × 150 mm or 21.2 mm × 150 mm) and a DAD detector. Fractions were monitored by TLC (GF 254, Qingdao Haiyang Chemical Co., Ltd. Qingdao), and spots were visualized by heating silica gel plates sprayed with 10% H₂SO₄ in EtOH.

UV spectra were obtained using a Shamashim UV 2401 spectrometer. Optical
rotations were recorded on a JASCO P-1020 polarimeter. IR spectra were measured on
a Bruker Tensor-27 infrared spectrophotometer with KBr pellets. HREIMS were
obtained on a Waters Autospec Premier P776 mass spectrometer. HRESIMS were taken
on an Agilent G6230 TOF MS spectrometer. 1D and 2D NMR spectra were recorded on
Bruker Avance-600 and Ultrashield-800 spectrometers using TMS as an internal
standard. Silica gel 200–300 mesh (Qingdao Marine Chemical Inc., China) and
Sephadex LH-20 (Amersham Biosciences, Sweden) were used for column chromatography.
Medium pressure liquid chromatography (MPLC) was performed on a Büchi Sepacore
System equipping pump manager C-615, pump modules C-605 and fraction collector
C-660 (Büchi Labortechnik AG, Switzerland), and columns packed with Chromatorex
C-18 (40–75 μm, Fuji Silysia Chemical Ltd., Japan). Preparative HPLC was performed
on an Agilent 1260 liquid chromatography system equipped with a Zorbax SB-C18
column (5 μm, 9.4 mm × 150 mm).