Sgw 533 automatic polarimeter

Melting points were obtained on a SGW X-4 micro melting point apparatus (INESA Co., Shanghai, China). Optical rotations were measured on a SGW-533 automatic polarimeter (INESA Co., Shanghai, China). The 1D and 2D NMR spectra were measured with a Bruker DRX-600 instrument (Bruker BioS-pin GmbH Company, Rheinstetten, Germany) with TMS as the internal standard. ESIMS data were recorded on an API QSTAR mass spectrometer (Applied Biosystem/MSD Sciex, Concord, Ontario, Canada); HRESIMS were recorded on a Waters Xevo G2-XS QTof mass spectrometer (USA). ECD spectra were recorded on a JASCO J-810 circular dichroism (CD) spectropolarimeter (JASCO Co., Tokyo, Japan). Column chromatography was performed on silica gel 60 (100–200 mesh, Qingdao Marine Chemical Ltd., Qingdao, China), sephadex LH-20 (GE Healthcare, Uppsala, Sweden), and Develosil ODS (50 μm, Nomura Chemical Co. Ltd., Osaka, Japan). The preparation of TLC was performed on HSGF254 plates (Jiangyou silicone Development Co., Ltd., Yantai, China).

Melting points were obtained on a SGW X-4 micromelting point apparatus (INESA Co., Shanghai, China). Optical rotations were measured on SGW-533 automatic polarimeter (INESA Co., Shanghai, China). HRESIMS spectra were taken on an API QSTAR mass spectrometer (Applied Biosystem/MSD Sciex, Concord, ON, Canada). The 1D- and 2D-NMR spectra were recorded on a Bruker Avance III 600MHz NMR spectrometer using TMS as an internal standard. Column chromatography was performed on silica gel (100–200 mesh, Qingdao Marine Chemical Ltd., Qingdao, China). Preparative TLC plates (HSGF254, Jiangyou silicone Development Co., Ltd., Yantai, China), Sephadex LH-20 (GE Healthcare, Uppsala, Sweden), and Develosil ODS (50 μm, Nomura Chemical Co. Ltd., Osaka, Japan) were used for the isolation experiments. Preparative HPLC was performed on a Waters 1525 Binary HPLC pump and a Waters 2414 refractive index detector (Waters Corp, Milford, MA, USA) using a YMC-Pack ODS-A column (250 mm ×10 mm I.D.; S-5 μm, 12 nm).