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4 protocols using 400mr ft nmr instrument

1

Analytical Techniques for Compound Characterization

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Optical rotations were determined with a JASCO P1020 digital polarimeter. IR spectra were taken on a JASCO FT/IR-4100 spectrometer. The NMR spectra were recorded on a Varian 400MR FT-NMR instrument at 400 MHz for 1H and 100 MHz for 13C, and on a Varian Unity INOVA 500 FT-NMR spectrometer at 500 MHz for 1H and 125 MHz for 13C in CDCl3. LR- and HR-ESIMS were measured with a Bruker APEX II mass spectrometer. Silica gel 60 (230–400 mesh, Merck, Darmstadt, Germany) and SiliaBond C18 silica gel (40–63 µm, 60 Å, 17% carbon loading, SiliCycle, Québec, QC, Canada) were used for column chromatography. Precoated silica gel plates (Kieselgel 60 F254, Merck, Darmstadt, Germany) and precoated silica gel RP-18 plates (Kieselgel 60 F254S, Merck, Darmstadt, Germany) were used for TLC analysis.
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2

Spectroscopic Characterization of Organic Compounds

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Optical rotations were measured on a Horiba High Sensitivity Polarimeter SEPA-300. Ultraviolet spectra were recorded on a JASCO V-650 spectrophotometer. IR spectra were recorded on a JASCO FT/IR-4100 infrared spectrophotometer. CD spectra were recorded on a JASCO J-815 CD spectrophotometer. NMR spectra were recorded on a Varian 400MR FT-NMR instrument at 400 MHz for 1H and 100 MHz for 13C in CDCl3. LRMS and HRMS were obtained by ESI on a Bruker APEX II mass spectrometer. Silica gel (Merck, 230–400 mesh) was used for column chromatography. Precoated silica gel plates (Merck, Kieselgel 60 F-254, 0.2 mm) were used for analytical TLC. High-performance liquid chromatography was performed on a Hitachi L-2455 HPLC apparatus with a Supelco C18 column (250 × 21.2 mm, 5 μm).
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3

Analytical Techniques for Chemical Characterization

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Optical rotations and IR spectra were recorded on a JASCO P-1020 polarimeter and FR/IR-4100 infrared spectrophotometer (Jasco Corporation, Tokyo, Japan), respectively. NMR spectra were acquired on a Varian Unity Inova 500 FT-NMR (Varian Inc., Palo Alto, CA, USA) at 500 and 125 MHz for 1H and 13C, respectively; or on Varian 400 MR FT-NMR instrument at 400 MHz and 100 MHz for 1H and 13C, respectively. The data of low-resolution electron spray ionization mass spectroscopy (LRESIMS) were measured by Bruker APEX II mass spectrometer. The data of HRESIMS were obtained by Bruker Apex-Qe 9.4T mass spectrometer. Silica gel 60 and reverse-phased silica gel (RP-18; 230–400 mesh) were used for normal-phase and reverse-phased column chromatography. Precoated silica gel plates (Kieselgel 60 F254, 0.2 mm) (Merck, Darmstadt, Germany) were used for analytical TLC. High-performance liquid chromatography was performed on a Hitachi L-2455 HPLC apparatus with a Supelco C18 column (ODS-3, 5 μm, 250 × 20 mm; Sciences Inc., Tokyo, Japan).
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4

Spectroscopic Characterization of Compounds

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Specific optical rotations were measured in CHCl3 using a JASCO P-1020 digital polarimeter (JASCO Corporation, Tokyo, Japan). IR spectra were recorded on a JASCO FT/IR-4100 spectrometer and an FT/IR-4100 infrared spectrophotometer (JASCO Corporation, Tokyo, Japan). The NMR experiments were performed in CDCl3 on a Varian 400MR FT-NMR instrument and a Varian Unity INOVA 500 FT-NMR spectrometer (Varian Inc., Palo Alto, CA, USA). LR- and HR-ESIMS were measured with a Bruker APEX II mass spectrometer and a Bruker Apex-Qe 9.4T mass spectrometer (Bruker, Bremen, Germany), respectively. Before column chromatography using Si gel or C18 gel (40–63 µm, Merck, Darmstadt, Germany), TLC analysis was performed on aluminum plates coated with Si gel or C18 gel (Kieselgel 60 F254, 0.25 mm, Merck, Darmstadt, Germany). HPLC was performed on a Hitachi L-2455 apparatus equipped with a Supelco C18 column (ODS-3, 5 μm, 250 × 20 mm; Sciences Inc., Tokyo, Japan).
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