Agilent 6540 q tof spectrometer

IR spectra were obtained on a Tenor 27 spectrometer with KBr pellets. ¹H and ¹³C NMR spectra were performed on AVANCE III-600 and AV 800 spectrometers with TMS as an internal standard (Bruker, Karlsruhe, Germany). ESIMS were run on an Agilent 6540 Q-TOF spectrometer (Agilent, Palo Alto, CA, USA). HR-EI-MS were run on an Shimadzu UPLC-IT-TOF spectrometer. HR-ESI-MS were measured using Agilent G6230 TOF MS (Agilent, Palo Alto, CA, USA). Semi-preparative HPLC was performed on an Agilent 1260 apparatus equipped with a diode-array detector and a Zorbax SB-C18 (Agilent, 9.4 mm × 25 cm) column. Column chromatography (CC) was performed using MCI gel (CHP 20P, 75–150 mm; Mitsubishi Chemical Corporation, Tokyo, Japan), silica gel (100–200 or 200–300 mesh, Qingdao Marine Chemical Co. Ltd., Qingdao, China) and Sephadex LH-20 (Amersham Pharmacia Biotech, Sweden). Thin-layer chromatography (TLC) was carried out on silica gel GF₂₅₄ on glass plates (Qingdao Marine Chemical Inc.) and spots were visualized by heating silica gel plates sprayed with 10% H₂SO₄ in EtOH. All reactions sensitive to air or moisture were carried out under argon or nitrogen atmosphere in dry and freshly distilled solvents under anhydrous conditions, unless otherwise noted.

UV spectra were measured using a Shimadzu UV-2401A spectrophotometer (Shimadzu, Tokyo, Japan). IR spectra were recorded on a Bruker Tensor 27 spectrophotometer (Bruker Optics, Ettlingen, Germany) with KBr pellets. 1D and 2D NMR spectra were carried out on Bruker AM-400 and DRX-500 or AVANCE III-600 and AV 800 spectrometers with TMS as an internal standard (Bruker, Karlsruhe, Germany). ESI-MS was run on an Agilent 6540 Q TOF spectrometer (Agilent, Palo Alto, CA, USA). HR-ESI-MS was performed using an Agilent G6230 TOF MS system (Agilent, Palo Alto, CA, USA). Semi-preparative HPLC was performed on an Agilent 1260 apparatus equipped with a diode-array detector and a Zorbax SB-C-18 (Agilent, 9.4 mm × 25 cm) column. Column chromatography was performed using MCI gel (CHP 20P, 75–150 mm; Mitsubishi Chemical Corporation, Tokyo, Japan), silica gel (100–200 or 200–300 mesh; Qingdao Marine Chemical Co. Ltd, Qingdao, China) and Sephadex LH-20 (GE Healthcare Bio-Sciences AB, Sala, Sweden). Thin-layer chromatography (TLC) was carried out on silica gel GF254 on glass plates (Qingdao Marine Chemical Inc.) and spots were visualized by heating silica gel plates sprayed with 10% H₂SO₄ in EtOH. All reactions sensitive to air or moisture were carried out under an argon or nitrogen atmosphere in dry and freshly distilled solvents under anhydrous conditions, unless otherwise noted.