Delta prep 4000 system

NMR spectra were recorded on a Bruker Avance III NMR spectrometer with the magnetic field of 11.74 Tesla. HR-ESI-MS were acquired on a Bruker Q-TOF mass spectrometer. Preparative HPLC was performed on a Waters Delta Prep 4000 system equipped with a Waters 2487 dual λ absorbance detector. A Rainbow Kromasil-C₁₈ (10 mm × 250 mm, 10 μm) column was selected for preparative HPLC. Column chromatography was performed on silica gel (160–200 mesh) and TLC analysis was carried on silica gel G plates (Qingdao Marine Chemical Plant, China). Sephadex LH-20 was purchased from Amersham Pharmacia Biotech (Beijing, China). MCI GELCHP20P (75–150 μm) was supplied by the Kaiteki Company (Tokyo, Japan). Analytical grade solvents were produced by Beijing Chemical Factory (Beijing, China).The deuterated solvents (CDCl₃, CD₃OD, DMSO-d₆, deuterated ratio, 99.8%) with TMS as the internal referent were produced by Cambridge Isotope Labo-ratories, Inc. (Andover, MA, USA).

NMR spectra were recorded on a Bruker Avance III 500 instrument (Bruker-Biospin, Billerica, MA, USA) at room temperature. Preparative HPLC was performed on a Waters Delta Prep 4000 system, which was equipped with a Waters 2487 dual λ absorbance detector. A Rainbow Kromasil-C₁₈ (10 mm × 250 mm, 10 μm) column was selected and performed for preparative HPLC. Column chromatography was performed on silica gel (160–200 mesh) and Thin Layer Chromatography (TLC) analysis was carried out on silica gel G plates (Qingdao Marine Chemical Plant, Qingdao, China). Sephadex LH-20 was purchase from Amersham Pharmacia Biotech (Beijing, China). Mitsubishi Chemical Ion (MCI) gel CHP20P (75–150 μm) was supplied by Kaiteki Company (Tokyo, Japan). All of the analytical reagents were purchased from Beijing Chemical Factory (Beijing, China). The deuterated solvents (CDCl₃, Deuterated ratio, 99.8%) with tetramethylsilane (TMS) were purchased from Cambridge Isotope Laboratories, Inc. (Andover, MA, USA).