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Advance 500 mhz nmr spectrometer

Manufactured by Bruker

The Bruker Advance 500 MHz NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It operates at a magnetic field strength of 500 MHz, providing high-resolution data for the structural elucidation and characterization of chemical compounds.

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7 protocols using advance 500 mhz nmr spectrometer

1

Characterization of Materials by Advanced Techniques

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Powder X-ray diffraction (PXRD) patterns were recorded using a D8 Advance diffractometer equipped with a LYNXEYE detector (Bragg–Brentano geometry, Cu Kα radiation λ = 1.54056 Å). Thermal gravimetric analysis (TGA) was performed using a TA Instruments Q-500 thermal gravimetric analyzer under airflow with a temperature ramp of 5 °C min−1. Fourier transform infrared (FT-IR) spectra were measured on a Bruker E400 FT-IR spectrometer using potassium bromide pellets. Low-pressure N2 and CO2 adsorption measurements were carried out on a Quantachrome Autosorb iQ volumetric gas adsorption analyzer. A liquid N2 bath was used for measurements at 77 K. Helium was used as an estimation of dead space. Ultrahigh-purity-grade N2, and He (99.999% purity) were used throughout adsorption experiments. Solution NMR spectra were recorded on a Bruker Advance-500 MHz NMR spectrometer. Scanning Electron Microscopy (SEM) images were performed on a JEOL JSM-75FCT. Gas chromatography (GC) analyses were performed using Agilent 6890 Series equipped with a flame ionization detector (FID) and a DB-5 column (length = 30 m, inner diameter = 320 μm, film thickness = 0.25 μm). GC-MS analyses were performed on Agilent GC System 7890 Series, equipped with a mass selective detector Agilent 5973N and a capillary DB-5MS column (length = 30 m, inner diameter = 320 μm, film thickness = 0.25 μm).
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2

Synthesis and Characterization of Amphiphilic Hyaluronic Acid Polymers

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Amphiphilic hyaluronic acid (HA) polymers were synthesized as described in previous reports.20 (link),26 (link) Briefly, 40-45 mg HA (MN = 10-20 kDa) was dissolved in 1:1 ultrapure water and DMF along with 30 mg of NHS and 30 mg of EDC. After mixing for 30 minutes to activate the HA carboxylic acid groups, 10 weight percent of hydrophobic reagent (octadecylamine or aminopropyl-pyrenebutanamide) was added to the HA solution and allowed to react for 24 hours. Samples were then removed and placed in 3500 MWCO dialysis tubing and dialyzed against 1:1 water and ethanol for 4 exchanges over 24 h, then against pure water for 8 exchanges over 48 h to remove any impurities. Finally, samples were frozen and freeze dried for later use. Structures of the obtained compounds were confirmed by 1H NMR spectroscopy on a Bruker Advance 500 MHz NMR spectrometer at 25°C (Figure S1-S2). Samples were analyzed in DMSO-d6 (99.9% D, Cambridge Isotope Laboratories). Data was processed in Mnova NMR (Escondido, CA). Hereafter, octadecyl-modified HA is referred to as ocdHA, and pyrene-butanamide substituted HA is referred to as pyHA.
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3

Macromonomer Synthesis Characterization by NMR

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1H-NMR was used to determine the successful synthesis of macromonomer materials. 1H-NMR spectroscopy was performed using a Bruker ADVANCE 500 MHz NMR spectrometer with deuterated chloroform ( CDCl3 ) as a solvent.
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4

Synthesis of 3-Hydroxychromone Derivatives

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All four derivatives of 3-hydroxychromone were synthesized following a two-stage Algar-Flynn-Oyamada procedure modified for better performance with electron donor-substituted aldehydes.19 To perform this technique, a corresponding aldehyde is reacted with 2-hydroxyacetophenone in DMF with addition of sodium methoxide to obtain a chalcone, which is subsequently subjected to an oxidative cyclization in ethanol with excess of sodium methoxide and 30% aqueous H2O2. Here, structures of the obtained compounds were confirmed by 1H NMR spectroscopy on a Bruker Advance 500 MHz NMR spectrometer at 25°C. Samples were analyzed in DMSO-d6 (99.9% D, Cambridge Isotope Laboratories). Data was processed in Mnova NMR (Escondido, CA). The synthetic details for each dye, as well the structure confirmation data are described in the Supplementary Information.
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5

Synthesis of Fluorescent Nucleosides

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Reactions were performed in flame-dried glassware under inert atmospheres (nitrogen or argon). Reactions were stirred using Teflon-coated stir bars. Solvents MeCN and CH2Cl2 were dried using an MBraun solvent purification system. Other solvents were purchased as ACS grade (≥99% purity) and used as received. Water for reactions and for photophysical characterization of the fluorescent nucleosides was purified using a MilliQ system (MilliporeSigma). 3,5-Di-O-toluoyl-α-1-chloro-2-deoxy-d-ribofuranose (12) was purchased from Carbosynth. Microwave reactions were performed on a Discover SP Microwave Synthesizer (CEM Corporation). Conditions used for microwave reactions were as follows: 17 bar, 200 watts, and 90 °C with stirring. Silica gel chromatography was performed using Redisep Rf high performance silica gel columns (Teledyne-Isco) on a Combiflash NextGen 300+ instrument (Teledyne-Isco). A Bruker Advance 500 MHz NMR spectrometer was used for the collection of all NMR spectra. NMR spectra were collected at room temperature. High resolution mass spectrometry was performed at the Analytical Biochemistry Core Facility at the University of Minnesota Masonic Cancer Center on an Exactive Plus Orbitrap mass spectrometer (Thermo Scientific).
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6

Quantitative NMR Analysis of PEG and Bottlebrush Polymers

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1H-NMR was used to determine successful synthesis of (1) the monofunctional PEG, (2) the difunctional PEG and (3) quantitative conversion of the M:I = 10 bottlebrush polymer. 1H-NMR spectroscopy was performed using a Bruker Advance 500 MHz NMR spectrometer with CDCl3 as a solvent.
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7

Characterization of Macromonomer Synthesis

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1H NMR was used to determine the successful synthesis of macromonomer materials (Figures S2 and S3). 13C NMR and ssNMR were used to determine the full conversion of closed-ring cross-linker norbornene to the open ring version seen in networks. NMR spectroscopy was performed by using a Bruker Advance 500 MHz NMR spectrometer with CDCl3 as a solvent (when needed).
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