1 H NMR spectra were obtained with either JEOL JNM-ECX500 (500 MHz) or JEOL ECA400 (400 MHz) spectrometers in deuterated solvents and tetrametylsilane was used as an internal standard. 13 C and DEPT NMR spectra were recorded in both instruments operating at 125 and 100 MHz, respectively. Meanwhile, two-dimensional NMR spectra, COSY, HMQC and HMBC were also measured by the JEOL JNM-ECX500 or JEOL ECA400 operating at 125 and 100 MHz, respectively. Infrared spectra were obtained by using the universal attenuated total reflection (UATR) technique on a Perkin -Elmer 100 Series FT -IR spectrometer. Mass spectra were recorded on a Shimadzu GCMS-QP5050A Plus spectrometer. Deuterated chloroform-d 1 (CDCl 3 ) was used in the analysis.
Jnm ecx500
Manufactured by JEOL
Sourced in Japan
The JNM-ECX500 is a compact and high-performance nuclear magnetic resonance (NMR) spectrometer designed for routine analytical applications. It provides a magnetic field strength of 500 MHz and is equipped with a superconducting magnet. The JNM-ECX500 is capable of conducting various NMR experiments and analyses, including proton (1H) and carbon-13 (13C) measurements.
Automatically generated - may contain errors
Lab products found in correlation
Su 8020 uhr, by Hitachi (1 mentions)
Ft ir 4200 spectrometer, by Jasco (1 mentions)
Gc 2025, by Shimadzu (1 mentions)
It 100 la, by JEOL (1 mentions)
Jem 1011 microscope, by JEOL (1 mentions)
Eca400, by JEOL (1 mentions)
Acetylthiocholine iodide, by Merck Group (1 mentions)
Apex 2 duo ccd diffractometer, by Bruker (1 mentions)
S butyrylthiocholine chloride, by Merck Group (1 mentions)
Tacrine, by Cayman Chemical (1 mentions)
Spectrum 100, by PerkinElmer (1 mentions)
Epoch 2, by Agilent Technologies (1 mentions)
5 5 dithiobis 2 nitrobenzoic acid, by Merck Group (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Tlc silica gel 60 f254, by Merck Group (1 mentions)
Hp 5ms, by Agilent Technologies (1 mentions)
Jnm ecz600r, by JEOL (1 mentions)
Merck silica gel 60 f254 plates, by Merck Group (1 mentions)
Jnm a400, by JEOL (1 mentions)
8 protocols using jnm ecx500
1
NMR and Spectroscopic Analysis of Compounds
2
Comprehensive Electrochemical and Spectroscopic Characterization
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A three-electrode configuration with a potentiostat/galvanostat/ZRA 3000 was used for voltammetric investigations (Gamry, USA). There was an Ag/AgCl reference electrode and an auxiliary electrode utilized, where the working electrodes were either bare or modified GCEs. The electrochemical studies were carried out in an electrolyte that had been nitrogen-purged prior to the experiment. Field emission scanning electron microscopy was utilized to study the material's morphology (FESEM, Hitachi SU 8020 UHR, Japan). The Agilent Cary 620/670 Series equipment was used in a Fourier transform infrared (FTIR) spectroscopy experiment that used the KBr disc method with an in-band wavelength range of 400 cm−1 to 4000 cm−1. inVia Raman spectroscopy was used to capture the Raman spectra, which were stimulated by a 514 nm Argon laser. Nuclear magnetic resonance spectroscopy was used to get 1H and 13C NMR spectra (NMR, JNM-ECX 500 JEOL, Japan).
3
NMR and Spectroscopic Characterization
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1H
NMR, 13C NMR, and 19F NMR spectra were recorded
on a JEOL JNM-ECX500 instrument (1H NMR: 500 MHz, 13C NMR: 126 MHz, 19F NMR: 471 MHz). The chemical
shift value by nuclear magnetic resonance (NMR) measurement was adjusted
based on the chloroform solvent signal (1H NMR: δ
7.26, 13C NMR: δ 77.0), the tetramethylsilane solvent
signal (TMS, 1H NMR: δ 0.00), or the hexafluorobenzene
solvent signal (19F NMR: δ −162.9). Coupling
constants in NMR spectra are abbreviated as s (singlet), d (doublet),
t (triplet), q (quartet), sep (septet), or m (complex multiplet).
The infrared (IR) absorption spectra were measured using a JASCO FT/IR-4200
spectrometer with the following relative intensities: s (strong),
m (medium), and w (weak). Mass spectra were measured using a JEOL
JMS-700 MStation or JMS-T100LP AccuTOF LC-plus 4G, DART/ESI/CSI/APCI.
The melting point was measured with MP-500D. Analytical gas chromatography
(GC) was performed on a SHIMADZU GC-2025 gas chromatograph with a
GL-Science capillary column (InterCap CHIRAMIX, id 0.25 mm ×
length 30 m, df 0.25 μm), equipped with a flame ionization detector.
MERCK Silica gel 60 was used for flash column chromatography. X-ray
crystallographic analysis was performed using a Rigaku VariMax RAPID
RA-Micro7HFM.
NMR, 13C NMR, and 19F NMR spectra were recorded
on a JEOL JNM-ECX500 instrument (1H NMR: 500 MHz, 13C NMR: 126 MHz, 19F NMR: 471 MHz). The chemical
shift value by nuclear magnetic resonance (NMR) measurement was adjusted
based on the chloroform solvent signal (1H NMR: δ
7.26, 13C NMR: δ 77.0), the tetramethylsilane solvent
signal (TMS, 1H NMR: δ 0.00), or the hexafluorobenzene
solvent signal (19F NMR: δ −162.9). Coupling
constants in NMR spectra are abbreviated as s (singlet), d (doublet),
t (triplet), q (quartet), sep (septet), or m (complex multiplet).
The infrared (IR) absorption spectra were measured using a JASCO FT/IR-4200
spectrometer with the following relative intensities: s (strong),
m (medium), and w (weak). Mass spectra were measured using a JEOL
JMS-700 MStation or JMS-T100LP AccuTOF LC-plus 4G, DART/ESI/CSI/APCI.
The melting point was measured with MP-500D. Analytical gas chromatography
(GC) was performed on a SHIMADZU GC-2025 gas chromatograph with a
GL-Science capillary column (InterCap CHIRAMIX, id 0.25 mm ×
length 30 m, df 0.25 μm), equipped with a flame ionization detector.
MERCK Silica gel 60 was used for flash column chromatography. X-ray
crystallographic analysis was performed using a Rigaku VariMax RAPID
RA-Micro7HFM.
4
Comprehensive Characterization of Novel Material
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Atomic force microscopy (AFM) images were obtained with a Digital Instrument Nanoscope III microscope with a tapping mode. X-ray diffraction (XRD) patterns were recorded with a Rigaku RINT-1000 diffractometer (Mn-filtered FeKα radiation) operating at a voltage of 40 kV, and a current of 30 mA, with a scan speed of 2.00° min−1, and a step width of 0.02°. Inductively coupled plasma (ICP) emission spectrometry experiments were performed using of a Varian VISTA MPX CCD Simultaneous ICP OES instrument. Proton nuclear magnetic resonance (NMR) was performed with a JEOL JNM-ECX500. A sample was dissolved in deuterated chloroform and measured. Scanning electron microscopy (SEM) images were acquired with a JEOL IT-100 LA. Transmission electron microscopy (TEM) images were obtained with JEOL JEM-1011 microscope operating at 100 kV. The sample was dropped onto a carbon grid and vacuum dried. Thermogravimetry was performed with a Thermo plus 8120/EVO2 equipment in the range 20–800 °C at a heating rate of 10.0 °C min−1 under an air flow.
5
Lipid Molecular Weight Analysis by MALDI-TOF MS
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The molecular weight of lipids was analyzed by Matrix Assisted Laser Desorption/Ionization Time of Flight Mass Spectrometry (MALDI-TOF MS) (AXIMA-CHR plus, Shimadzu) with 2,5dihydroxybenzoic acid (Fujifilm Wako Pure Chemical) as a matrix material. Positive ions were detected with reflectron mode. Samples were solubilized in CDCl 3 / CD 3 OD (2:1, v/v), and 1 H-Nuclear Magnetic Resonance (NMR) was measured using the equipment JNM-ECX 500 (500 MHz, JEOL RESONANCE) at 45°C.
6
Synthesis and Characterization of Xanthone Derivatives
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The solvents (analytical grade), silica gel 60, and thin-layer chromatography (TLC) silica gel 60 F254 were obtained commercially from Merck (United States). The chemicals and reagents used in the synthesis reactions were obtained from Sigma Aldrich (Germany) with high purity (>95%). Acetylcholinesterase from Electrophorus electricus (500 UN), butyrylcholinesterase from Equine serum (1.2 KU), acetylthiocholine iodide, S-butyrylthiocholine chloride, and 5,5′-Dithiobis (2-nitro benzoic acid) were obtained from Sigma Aldrich. Tacrine (Purity >98%) was obtained from Cayman Chemical. The melting point of derivatives was determined by Electrothermal 9100 Series Apparatus. Mass spectra of derivatives were acquired from Gas Chromatography-Mass Spectrometry (GCMS) (Agilent J&W) equipped with GC column HP-5MS (30 m × 0.25 mm × 0.25 µm). 1H and 13C NMR spectral data of derivatives were obtained from JEOL JNM-ECX 500 or JNM-ECZ 600 R NMR spectrometers. FTIR spectra of derivatives were recorded on Perkin Elmer Spectrum 100 (Perkin Elmer) equipped with attenuated total reflection (ATR). X-ray analysis was performed using Bruker APEX II DUO CCD diffractometer. Optically active xanthones were analysed using polarimeter Optika POL-1 bench polarimeter. The absorbance of the biological assay was measured with microplate reader BioTek Epoch 2.
7
Trichothecene Conjugates Characterization
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All NMR spectra were recorded on a JEOL JNM-ECX500 (500 MHz) spectrometer in deuterated methanol (MeOH-d3) calibrated with a solvent peak at 3.31 ppm for the measurement of H nucleus and 49.3 ppm for that of C nucleus. Purified trichothecenes conjugates were identified by some analyses of 1H NMR, 13C NMR, correlation spectroscopy (COSY), heteronuclear multiple quantum coherence (HMQC), and heteronuclear multiple bond coherence (HMBC). If necessary, total correlation spectroscopy (TOCSY) or 1D-nuclear overhauser effect (1D-NOE) analysis was performed.
8
General Synthetic Procedures and Characterization Data
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Chemicals were purchased from Sigma–Aldrich, Merck (Darmstadt, Germany), FUJIFILM Wako Chemicals (Osaka, JAPAN), Nacalai Tesque, Tokyo Chemical Industry (Tokyo, Japan), and Kanto Chemical (Tokyo, Japan) and used without further purification. Column chromatography was done on Cica silica gel 60N (spherical, neutral; particle size, 63–210 nm, Kanto Chemical), while thin-layer chromatography was performed using Merck silica gel 60F254 plates. Melting points were taken on a Yanaco micromelting point apparatus and are uncorrected. The nuclear magnetic resonance (NMR) spectra were acquired in the specified solvent in JEOL JNM-A400 (400 and 100 MHz for 1H and 13C, respectively) or JEOL JNM-ECX500 (500 and 125 MHz for 1H and 13C, respectively). The chemical shifts (δ) are reported in ppm downfield from TMS, and coupling constants (J) are expressed in Hertz. IR spectra were measured with a JASCO FT/IR-460 Plus spectrophotometer (JASCO Corp., Tokyo, Japan). The low-resolution and high-resolution mass spectra were obtained with a Shimadzu GCMS-QP 500 mass spectrometer (Shimadzu Corp., Kyoto, Japan), JEOL D-200, or JEOL AX505 mass spectrometer (JEOL Ltd., Tokyo, Japan) in the electron impact mode at the ionization potential of 70 eV.
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