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Avance dpx 500

Manufactured by Bruker
Sourced in United States

The Avance DPX-500 is a nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It operates at a magnetic field strength of 500 MHz and is designed for high-resolution NMR spectroscopy. The core function of the Avance DPX-500 is to provide researchers and analytical laboratories with a reliable and high-performance tool for the structural analysis and characterization of chemical compounds.

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10 protocols using avance dpx 500

1

Synthesis of Pyridinone-Based Compounds

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All reagents and solvents were of general purpose or analytical grade and purchased from Sigma-Aldrich Ltd, Fisher Scientific, Fluka and Acros. 1H, 13C and 19F NMR spectra were recorded with a Bruker Avance DPX500 spectrometer operating at 500, 125 and 470 MHz respectively, with Me4Si as internal standard. Elemental analysis was performed (for compounds 10e and 10g) by MEDAC Ltd (Chobham, Surrey, UK). High resolution mass spectra (HRMS) were determined (for compounds 9a–j, 10a–d, 10f, and 10h) at the EPSRC National Mass Spectrometry Facility at Swansea University and Medac Ltd (Chobham, Surrey, UK), using ESI (Electrospray Ionisation). Flash column chromatography was performed with silica gel 60 (230–400 mesh) (Merck) and TLC was carried out on precoated silica plates (kiesel gel 60 F254, BDH). Compounds were visualised by illumination under UV light (254 nm). Melting points were determined on an electrothermal instrument and are uncorrected. All solvents were dried prior to use and stored over 4 Å molecular sieves, under nitrogen. All the compounds were ≥95% pure.
The following compounds were prepared as previously described: PCV (6),16 HBG (7),17 (link) and the bromoketones (8).21 , 22 (link), 23 , 24 (link), 25 (link)
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2

C-13 NMR Analysis of Polysaccharides

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13C NMR spectra were obtained on an Avance DPX-500 NMR spectrometer (Bruker BioSpin Corporation, Billerica, MA, USA) at 35 °C with acetone as the internal standard (pulse sequence—zgpg, flip angle—90°, scans—128, relaxation delay—1.5 s, and acquisition time—0.38 s). The sample concentration was 15 mg of polysaccharide per 600 mL of D2O.
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3

Synthesis of Heterocyclic Compounds

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All reagents and solvents were of
general purpose or analytical grade and purchased from Sigma-Aldrich
Ltd., Fisher Scientific, Fluka, and Acros. 1H and 13C NMR spectra were recorded with a Bruker Avance DPX500 spectrometer
operating at 500 and 125 MHz, with Me4Si as an internal
standard. Mass spectra (HRMS) were determined by the EPSRC mass spectrometry
center (Swansea, UK). Elemental analysis was performed by MEDAC Ltd.
(Chobham, Surrey, UK). Flash column chromatography was performed with
silica gel 60 (230–400 mesh) (Merck), and TLC was carried out
on precoated silica plates (kiesel gel 60 F254, BDH). Compounds
were visualized by illumination under UV light (254 nm) or by the
use of vanillin stain followed by heating. Melting points were determined
on an electrothermal instrument and were uncorrected. All solvents
were dried prior to use and stored over 4 Å molecular sieves,
under nitrogen. All of the compounds were ≥95% pure.
The imines (3), aldehydes (4), alcohols
(5), chlorides (6), carboxylic acids (9), and 1-(2-ammonioethyl)-1H-imidazol-3-ium
chloride (12) were prepared as previously described.9 (link)−13 (link) All compounds were more than 95% pure.
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4

Synthesis and Characterization of Organic Compounds

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All reagents and solvents were of general
purpose or analytical grade and were purchased from Sigma-Aldrich
Ltd., Fisher Scientific, Fluorochem, or Acros. 1H and 13C NMR data were recorded on a Bruker AVANCE DPX500 spectrometer
operating at 202, 500, and 125 MHz. Chemical shifts (δ) are
quoted in ppm, and J values are quoted in Hz. In
reporting spectral data, the following abbreviations were used: s
(singlet), d (doublet), t (triplet), q (quartet), dd (doublet of doublets),
td (triplet of doublets), and m (multiplet). All of the reactions
were carried out under a nitrogen atmosphere and were monitored using
analytical thin-layer chromatography on precoated silica plates (Kieselgel
60 F254, BDH). Compounds were visualized by illumination under UV
light (254 nm) or by the use of KMnO4 stain followed by
heating. Flash column chromatography was performed with silica gel
60 (230–400 mesh) (Merck). High-performance liquid chromatography
(HPLC) was carried out on a SHIMADZU Prominence-i quaternary low-pressure
gradient pump with a Prominence-i UV detector (190 to 700 nm). All
solvents for HPLC were of HPLC grade and purchased from Fisher Scientific.
HPLC data analysis was performed using the SHIMADZU Lab Solutions
software package. The purity of the final compounds was determined
by HPLC, and they were all of ≥95% purity unless stated otherwise.
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5

NMR and IR Analysis of Organic Compounds

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IR spectra were recorded using a Perkin-Elmer 1000 spectrophotometer. 1H and 13C NMR were recorded on a Bruker Avance DPX-500 (500 MHz for 1H and 125 MHz for 13C); chemical shifts are given in ppm (δC and δH) relative to CDCl3 (7.27) and (77.23).
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6

Analytical Characterization of Carp Swim Bladder

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All reagents and materials were purchased from commercial sources
and used without purification. All of them were analytical grade.
The swim bladders were obtained from common carp of Caspian Sea. SEM
analysis was performed by using KYKY-EM3200 (26 kV). TEM analysis
was carried out by EM10C-100 kV. XRD analysis was done by Holland
Philips Xpert, Co K and ultrasonicated by Topsonics, 20 KHz, 400 W. 1H and 13C NMR spectra were recorded on Bruker AVANCE
DPX 500. The chemical shifts (δ) are given in parts per million
and referenced to the tetramethylsilane internal standard. IR spectra
were recorded in KBr on a Shimadzu FT-IR spectrometer and were reported
in wavenumbers (cm–1). All melting points were measured
on a capillary melting point apparatus.
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7

NMR Analysis of Lacebark Mucilage

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Lacebark mucilage was exchanged with deuterium by freeze-drying with D2O (99.9 atom%) three times. Samples were dissolved in D2O and 1 H and 13 C (both 1 H coupled and decoupled) spectra were recorded on a Bruker Avance DPX-500 spectrometer at 90C. The 1 H and 13 C chemical shifts were measured relative to an internal standard of (CH3)2SO ( 1 H, 2.70 ppm; 13 C, 39.5 ppm; [23] ). Assignments were made from heteronuclear single quantum coherence (HSQC) COSY experiments and by comparing the spectra with published data.
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8

Purification and Characterization of Novel Compounds

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All the reagents used were commercial and were used without further purification unless specifically stated. Analyticalthin-layer chromatography and preparative thin-layer chromatography were performed with silica gel plates using silica gel 60 GF254 (Qingdao Haiyang Chemical Co., Ltd., Qingdao, Shandong Province, China) . The separation of certain compounds was accomplished by using reverse-phase preparative HPLC (Gilson ODS-BP) with a UV detector at 254 nm as described in further detail in the Supporting Information. Melting points were determined using WRS-1B digital melting point apparatus. NMR spectra were measured on a Bruker Avance-DPX500, chemical shifts are shown in δ values (ppm) with tetramethylsilane (TMS) as internal standard. ESI-MS were obtained using Agilent 1100 Series instrument. Single crystal X-ray diffraction was on a Bruker AXS D8 QUEST X-ray single crystal diffractometer. Purity of the compounds was confirmed to be ≥97% by HPLC.
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9

General Organic Synthesis Protocols

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General information. All reagents and solvents were of general purpose or analytical grade and were purchased from Sigma-Aldrich Ltd. (Merck), Fisher Scientific, Fluorochem, or Acros. 31 P, 1 H, 19 F and 13 C NMR data were recorded on a Bruker AVANCE DPX500 spectrometer operating at 202, 500, and 125 MHz, respectively. Chemical shifts (δ) are quoted in ppm, and J values are quoted in Hz. In reporting spectral data, the following abbreviations were used: s (singlet), d (doublet), t (triplet), q (quartet), dd (doublet of doublets), td (triplet of doublets), and m (multiplet). All of the reactions were carried out under a nitrogen atmosphere and were monitored using analytical thin layer chromatography on precoated silica plates (kiesel gel 60 F254, BDH). Compounds were visualized by illumination under UV light (254 nm) or by the use of KMnO4 stain followed by heating. Flash column chromatography was performed with silica gel 60 (230-400 mesh) (Merck). HPLC was carried out on a SHIMADZU Prominence-i quaternary lowpressure gradient pump with a Prominence-i UV detector (190 to 700 nm). All solvents for HPLC were HPLC grade purchased from Fisher Scientific. HPLC data analysis was performed using the SHIMADZU Lab solutions software package. The purity of the tested prodrugs was determined by HPLC, and they were all of ≥95% purity, except where specified.
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10

NMR Analysis of Lacebark Mucilage

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Lacebark mucilage was exchanged with deuterium by freeze-drying with D2O (99.9 atom%) three times. Samples were dissolved in D2O and 1 H and 13 C (both 1 H coupled and decoupled) spectra were recorded on a Bruker Avance DPX-500 spectrometer at 90C. The 1 H and 13 C chemical shifts were measured relative to an internal standard of (CH3)2SO ( 1 H, 2.70 ppm; 13 C, 39.5 ppm; [23] ). Assignments were made from heteronuclear single quantum coherence (HSQC) COSY experiments and by comparing the spectra with published data.
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