General Remarks All reagents and solvents purchased were of the highest commercial quality and were used without further purification. 1 H-NMR spectra were measured at 400 MHz on a VARIAN 400-MR spectrometer or at 500 MHz on an Agilent INOVA-500 spectrometer, and 13 (link) C-NMR spectra were measured at 100 MHz on a VARIAN 400-MR spectrometer or at 125 MHz on an Agilent INOVA-500 spectrometer. High resolution mass spectra were recorded using a Jeol JMS-T100LP AccuTOF instrument. IR spectra were recorded using a JASCO FT/IR-4700 spectrometer in attenuated total reflection (ATR) mode at room temperature. Silica gel column chromatography was performed using Silica Gel 60 (spherical and neutral; 100 to 210 µm, 37560-79, Kanto Chemical Co., Japan) and the Isolera One flash purification system (Biotage, Sweden). After stirring overnight at reflux temperature, the reaction mixture was concentrated under reduced pressure. The residue was dissolved in AcOEt (60 mL), and the solution was washed with water (40 mL×2) and brine (40 mL). The organic layer was dried over Na 2 SO 4 , filtered, and concentrated under reduced pressure. The resulting residue was purified using the Isolera One system (hexane/ AcOEt) to afford 16 as a yellow oil (4435 mg, 81%).
400 mr spectrometer
Manufactured by Agilent Technologies
Sourced in United States, Canada
The 400-MR spectrometer is a laboratory instrument designed for nuclear magnetic resonance (NMR) analysis. It provides a core function of acquiring and processing NMR data to identify and characterize chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
Prominence hplc, by Shimadzu (6 mentions)
Nicolet 6700, by Thermo Fisher Scientific (3 mentions)
Onenmrprobe pt probe head, by Agilent Technologies (2 mentions)
Xevo tq s mass spectrometer, by Waters Corporation (2 mentions)
Inova 500 spectrometer, by Agilent Technologies (2 mentions)
Q tof 1200 series, by Agilent Technologies (2 mentions)
Uv 2450, by Hitachi (1 mentions)
Ft ir spectrum rx 1, by PerkinElmer (1 mentions)
F 7000 spectrophotometer, by Hitachi (1 mentions)
Mpms xl 5 squid magnetometer, by Quantum Design (1 mentions)
Q tof premier mass spectrometer, by Waters Corporation (1 mentions)
Vnmrs 500, by Agilent Technologies (1 mentions)
Hplc system, by Shimadzu (1 mentions)
Bas 5000 phosphorimager, by Fujifilm (1 mentions)
Combiflash rf 200, by Teledyne (1 mentions)
Sta 449f3 instrument, by Netzsch (1 mentions)
Jsm 7500f scanning electron microscope, by JEOL (1 mentions)
Uv 2550 uv vis spectrometer, by Shimadzu (1 mentions)
Luna c18 column, by Phenomenex (1 mentions)
Microtof q 2 mass spectrometer, by Bruker (1 mentions)
42 protocols using 400 mr spectrometer
1
Purification and Characterization of Organic Compound
2
NMR Analysis of Nucleotide Samples
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All NMR experiments were conducted on a Varian 400-MR spectrometer (9.4 T, 400 MHz). Samples were prepared by re-suspending evaporated nucleotide samples in 500 μL D2O supplemented with 5 mM TMSP (3-(trimethylsilyl)propionic-2,2,3,3-d4) at 27 °C. Data were processed and figures were generated using VnmrJ software (version 2.2C). 1H and 31P chemical shifts are reported in parts per million (ppm). J coupling constants are reported in units of frequency (Hertz) with multiplicities listed as s (singlet), d (doublet), and m (multiplet). These data appear in the figure legends of each NMR spectra.
3
NMR Analysis of Nucleotide Samples
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All NMR analyses were conducted on a Varian 400-MR spectrometer (9.4 T, 400 MHz) as previously described (Whiteley et al., 2019 (link)). Samples were prepared by resuspending evaporated nucleotide samples in 500 μL D2O supplemented with 0.75% TMSP (3-(trimethylsilyl)propionic-2,2,3,3-d4) at 27°C. VnmrJ software (version 2.2C) was used to process data and generate figures. 1H and 31P chemical shifts are reported in parts per million (p.p.m.). J coupling constants are reported in units of frequency (Porritt and Hertzog) with multiplicities listed as s (singlet), d (doublet) and m (multiplet). These data appear in the figure legends of each NMR spectrum.
4
Structural Characterization of Polysaccharide
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A FT-IR Spectrum RX 1 (PerkinElmer) was employed to acquire the Fourier Transform−Infrared spectrum in the frequency scale of 400–4000 cm−1. For analysis, lyophilised polysaccharide (P ) ground with KBr (1:20) was utilised for pellet assembling. Ultraviolet-visible and fluorescence spectra were acquired on Shimadzu UV-2450 and Hitachi F−7000 spectrophotometer, respectively. The 1H NMR spectrum of fraction P was obtained via a Varian 400MR spectrometer at 25 °C. The hydroxylic protons of polysaccharide sample (10 mg) were replaced with deuterium using 99.9% D2O (Sigma Aldrich) and this process repeated thrice to diminish the signal residual proton. This deuterium exchanged sample was dissolved in 500 μL D2O for subsequent proton NMR measurement. The electrospray ionization mass spectrum of per-O-acetylated oligomers (O ) was acquired by means of a QTOF 60 Micro YA 263 mass spectrometer.
5
Synthesis and Characterization of Azine Complexes
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All chemicals and solvents used for syntheses of azine compounds and Ni complexes were reagent grade and used without further purification. First, 2-pyridinecarboxaldehyde, 1H-imidazole-4-carboxaldehyde, 2-methyl-1H-imidazole-4-carboxaldehyde, nickel(II) chloride hexahydrate, and ammonium hexafluorophosphate were purchased from FUJIFILM (Tokyo, Japan). All reactions were carried out under aerobic conditions. Infrared spectra (KBr pellets; 4000–400 cm−1) were recorded on a JASCO FT-001 Fourier transform infrared spectrometer (JASCO, Tokyo, Japan). Absorption spectra were recorded on a Shimadzu UV/Vis-1650 spectrophotometer (Kyoto, Japan) in the range of 200–600 nm at room temperature in acetonitrile. The 1H NMR spectra were acquired on a Varian 400-MR spectrometer (Los Angeles, CA, USA); the chemical shifts were referenced to residual 1H NMR signals of solvents and are reported versus TMS. Elemental analyses were conducted at Advanced Science Research Center, Okayama University. Magnetic susceptibilities were measured on a Quantum Design MPMS XL5 SQUID magnetometer (Tokyo, Japan) in a 1.9–300 K temperature range under an applied magnetic field of 0.1 T at the Okayama University of Science. Corrections for diamagnetism were applied using Pascal’s constants [35 (link)].
6
Synthesis and Characterization of Compounds 1-4
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All chemicals for synthesis were purchased from Alfa Aesar (Ward Hill, MA) or Aldrich (Milwaukee, WI). The compound identity was characterized by 1H NMR on a Varian (Palo Alto, CA) 400-MR spectrometer. The purities of synthesized compounds were determined by a Shimadzu Prominence HPLC with a Zorbax C18 (or C8) column (4.6 × 250 mm) monitored by UV at 254 nm. The purities of the reported compounds were found to be >95 %. Synthesis and characterization of compounds 1 –4 can be found in Additional file 1 .
7
Synthesis and Characterization of Compounds 1-5
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Compounds 1 – 5 were synthesized using the published methods [49 (link), 17 (link), 50 , 51 (link), 40 (link)] and characterized by 1H and 13C NMR on a Varian (Palo Alto, CA) 400-MR spectrometer, showing identical NMR spectra to those reported. The compound purities were determined by a Shimadzu Prominence HPLC with a Zorbax C18 column (4.6 × 250 mm) monitored by UV absorbance at 254 nm. The purities of all compounds were found to be >95%.
8
Comprehensive Characterization of Organic Compounds
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All solvents and
reagents were used as obtained from commercial sources unless otherwise
indicated. Commercial reagents and anhydrous solvents were used without
further purification. Analytical thin layer chromatography (TLC) was
performed on silica gel 60 F254 aluminum sheets. Removal of solvents
was conducted by using a rotary evaporator, and residual of solvents
was removed from nonvolatile compounds using a vacuum manifold. All
reported yields are isolated yields. 1H and 13C NMR spectra were recorded on a Varian 400MR spectrometer operating
at 400 MHz for 1H and 100 MHz for 13C. Deuterated
dimethyl sulfoxide or deuterated methanol or deuterated chloroform
was used as the solvent for NMR experiments. 1H chemical
shift values (δ) are referenced to the residual nondeuterated
components of the NMR solvents (δ = 2.54 ppm for DMSO, δ
= 7.26 ppm for CDCl3, and δ = 3.31 ppm for CD3OD). The 13C chemical shifts (δ) are referenced
to CDCl3 (central peak, δ = 77.16 ppm) or CD3OD (δ = 49.00 ppm) as the internal standard. The HRMS
data were obtained on a Waters Q-TOF Premier mass spectrometer. Column
chromatography was performed using silica gel (35–75 mesh).
The purity of final compounds was evaluated by C, H, N analysis (Atlantic
Microlabs). The purity of all the final compounds was confirmed to
be ≥95% by combustion.
reagents were used as obtained from commercial sources unless otherwise
indicated. Commercial reagents and anhydrous solvents were used without
further purification. Analytical thin layer chromatography (TLC) was
performed on silica gel 60 F254 aluminum sheets. Removal of solvents
was conducted by using a rotary evaporator, and residual of solvents
was removed from nonvolatile compounds using a vacuum manifold. All
reported yields are isolated yields. 1H and 13C NMR spectra were recorded on a Varian 400MR spectrometer operating
at 400 MHz for 1H and 100 MHz for 13C. Deuterated
dimethyl sulfoxide or deuterated methanol or deuterated chloroform
was used as the solvent for NMR experiments. 1H chemical
shift values (δ) are referenced to the residual nondeuterated
components of the NMR solvents (δ = 2.54 ppm for DMSO, δ
= 7.26 ppm for CDCl3, and δ = 3.31 ppm for CD3OD). The 13C chemical shifts (δ) are referenced
to CDCl3 (central peak, δ = 77.16 ppm) or CD3OD (δ = 49.00 ppm) as the internal standard. The HRMS
data were obtained on a Waters Q-TOF Premier mass spectrometer. Column
chromatography was performed using silica gel (35–75 mesh).
The purity of final compounds was evaluated by C, H, N analysis (Atlantic
Microlabs). The purity of all the final compounds was confirmed to
be ≥95% by combustion.
9
Spectroscopic Characterization of Molecular Structures
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For structure elucidation 1H, 13C, gCOSY, gNOESY, gHSQC and gHMBC NMR spectra were acquired on an Bruker Avance III HD 800 MHz, on a Varian VNMR-S 500 or a Varian 400 MR spectrometer. The spectra were processed using the MestReNova (v9.0.0) software. Chemical shifts were referenced indirectly to tetramethylsilane via the residual solvent signal (CHCl3, 1H at 7.26 ppm and 13C at 77.16 ppm). LC(ESI)MS spectra was acquired on a PE SCIEX API 150EX instrument (Perkin Elmer, Waltham, MA, USA) equipped with a Turbolon spray ion source (30 eV ionization energy) and a Gemini 5 mmC-18 110 Å HPLC column, using water:acetonitrile gradient (80:20 to 20:80).
10
Characterization of Synthesized Compounds
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Example 1
All chemicals for synthesis were purchased from Alfa Aesar (Ward Hill, Mass.) or Aldrich (Milwaukee, Wis.). The compound identity was characterized by 1H NMR on a Varian (Palo Alto, Calif.) 400-MR spectrometer. The purities of synthesized compounds were determined by a Shimadzu Prominence HPLC with a Zorbax C18 (or C8) column (4.6—250 mm) monitored by UV at 254 nm. The purities of the reported compounds were found to be >95%.
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