Amx 500 instrument

Optical rotations were recorded on a Perkin-Elmer model 341 polarimeter (Perkin-Elmer Inc., Waltham, MA, USA). The UV and CD spectra were recorded on a UV-8000 spectrophotometer (Shanghai Metash instruments Co., Ltd., Shanghai, China) and a Jasco J-715 spectropolarimeter in MeOH (JASCO, Tokyo, Japan), respectively. The IR spectra were obtained on a VERTEX 70v FT-IR spectrometer (Bruker Biospin Corp., Billerica, MA, USA). The NMR experiments were conducted on a Bruker AMX-500 instrument (Bruker Biospin Corp., Billerica, MA, USA). HRESIMS spectra were recorded on an AB SCIEX Triple Tof-4600 spectrometer (ABSciex, Vaughan ON, Canada). Column chromatographic separations were carried out using silica gel (200–300 mesh, Qingdao Ocean Chemical Co., Ltd., Qingdao, China) and ODS (50 μm, YMC Co., Ltd., Kyoto, Japan). MPLC was carried out on a SepaBean machine (Santai Technology Co., Ltd., Changzhou, China). RP HPLC was performed on a YMC-Pack Pro C18 column (250 × 10 mm, 5 mm, YMC Co., Ltd., Kyoto, Japan) using a Waters 1525 binary HPLC pump with a Waters 2998 photodiode array detector (Waters Corp., Milford, MA, USA). Analytical thin-layer chromatography was performed on silica gel HSGF254 plates and visualized by spraying with anisaldehyde–H₂SO₄ reagent.

Nuclear magnetic resonance (NMR) were performed on a Bruker AMX 500 instrument (Billerica, MA) with standard pulse sequences operating at 500 MHz in ¹H NMR and 125 MHz in ¹³C NMR, chemical shifts are given in δ values (ppm) using tetramethylsilane as the internal standard and DMSO-d₆ as solvent at room temperature and coupling constants were reported in Hz. Infra-red (IR) spectra were recorded with Nexus 670 FT-IR FT-Ramen spectrometer (Gaithersburg, MD) as potassium bromide discs. UV spectra were recorded with Shimadzu UV-1601 (Kyoto, Japan). HRESI-MS was taken on a Micromass Autospec (70 eV) spectrometer. Column chromatography was performed on polyamide 6 and Sephadex LH-20.

Optical rotation data were recorded on a PerkinElmer model 341 polarimeter with a 10 cm length cell at room temperature. UV and IR (KBr) spectra were obtained on a Hitachi U-3010 spectrophotometer and Jasco FTIR-400 spectrometer, respectively. CD spectra were obtained on a Jasco J-715 spectropolarimeter in MeCN. NMR spectra including 1D and 2D spectra were acquired at room temperature on Bruker AMX-500 instrument. HRESIMS data were obtained on a Waters Q-Tof micro YA019 mass spectrometer. Reversed-phase HPLC was performed on YMC-Pack Pro C18 RS (5 μm) columns with a Waters 1525 separation module equipped with a Waters 2998 photodiode array detector. Purifications by column chromatography were performed on silica gel 60 (200–300 mesh; Yantai, China), Sephadex LH-20 (18–110 μm, Pharmacia Co.), and ODS (50 μm, YMC Co.). Analytical thin-layer chromatography was carried out using HSGF 254 plates and visualized by spraying with anisaldehyde-H₂SO₄ reagent.