Ultimate 3000

Optical rotations were measured in MeOH on a P-1020 polarimeter (JASCO, Tokyo, Japan). UV spectra were obtained on a 2401PC spectrophotometer (Shimadzu Co., Tokyo, Japan), while 1D and 2D NMR spectra were recorded on a Bruker AVANCEIII-500 MHz spectrometer (Bruker, Ettlingen, Germany) in acetone-d₆, CD₃OD, and C₅D₅N using tetramethylsilane (TMS) as an internal reference standard. Chemical shifts were expressed as δ in ppm and the coupling constants (J) were given in Hz. High-resolution electrospray mass spectroscopy was performed on an Agilent G6230 TOF mass spectrometer (HR-ESI-MS) (Agilent Technologies, California, CA, USA) and a Waters Autospec Premier 776 mass spectrometer (HR-EI-MS) (Waters Technologies, Massachusetts, MA, USA). High-performance liquid chromatography (HPLC) was conducted on an Ultimate 3000 HPLC system (Dionex Co., Sunnyvale, CA, USA) equipped with an Ultimate 3000 pump and variable wavelength detector, as well as a semi-preparative YMC-Pack ODS-A column (250 × 10 mm, 5 µm, YMC, Kyoto, Japan). Column chromatography (CC) was conducted over silica gel (300–400 mesh, Qingdao Haiyang Co. Ltd., Qingdao, China). HPLC grade methanol and acetonitrile were purchased from Tedia Co. Inc, (Fairfield, OH, USA).

The 1D and 2D NMR spectra were recorded on a Bruker AVANCE Ⅲ-500 MHz and a Bruker AV-400 MHz spectrometer (Bruker, Ettlingen, Germany) in pyridine-d₅ or acetone-d₆ using tetramethyl silane (TMS) as an internal reference standard. Chemical shifts (δ) are expressed in ppm, and the coupling constants (J) are given in Hz. High-resolution electrospray mass spectroscopy was performed on a Waters Autospec Premier 776 mass spectrometer (HR-EI-MS) (Waters Technologies, Milford, MA, USA) and an Agilent G6230 TOF mass spectrometer (HR-ESI-MS) (Agilent Technologies, Santa Clara, CA, USA). High-performance liquid chromatography (HPLC) was conducted on an Ultimate 3000 HPLC system (Thermo Fisher, Waltham, MA, USA) equipped with an Ultimate 3000 pump and Ultimate 3000 variable wavelength detector, as well as a semi-preparative YMC-Pack ODS-A column (250 × 10 mm, 5 μm) from YMC Co. Ltd. (Kyoto, Japan), column chromatography (CC) was conducted over silica gel (200–300 mesh and 300–400 mesh, Qingdao Haiyang Chemical Industry, Qingdao, China). Chromatographic grade methanol and acetonitrile were purchased from Tedia Co. Inc. (Fairfield, OH, USA).