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300 mhz mercury spectrometer

Manufactured by Bruker

The 300 MHz Mercury Spectrometer is a nuclear magnetic resonance (NMR) instrument produced by Bruker. It operates at a magnetic field strength of 7.05 Tesla, corresponding to a resonance frequency of 300 MHz for hydrogen nuclei (1H). The core function of this spectrometer is to provide high-resolution NMR analysis of samples.

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5 protocols using 300 mhz mercury spectrometer

1

Analytical Characterization of Organic Compounds

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All reagent-grade chemicals were obtained from commercial suppliers and were used without further purification. Reactions were monitored by thin-layer chromatography (TLC) on aluminum-backed sheets with silica gel 60 GF254 (HX805651) and a fluorescent indicator (visualized with UV light of 254 nm). Flash chromatography was performed using silica gel 60 (230–400 mesh). Melting points (mp) were determined on an Electrothermal IA 91000 apparatus (Electrothermal, Bibby Scientific, Staffordshire, ST15 OSA, UK) and were uncorrected. 1H and 13C NMR spectra were obtained on a Varian Mercury 300 MHz spectrometer or a Bruker Avance III 750 MHz spectrometer using deuterated dimethyl sulfoxide (DMSO-d6) or deuterated chloroform (CDCl3) as the solvent and tetramethylsilane (TMS) as the internal standard. Chemical shifts (δ) are reported in ppm downfield from the internal standard, and coupling constants are reported in Hertz (Hz) (Supplementary Material). Electrospray ionization high-resolution mass spectrometry positive mode (ESI-HRMS) was performed with an Agilent 6545 QTOF LC/MS instrument (Agilent Technologies, Santa Clara, CA, USA).
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2

Spectroscopic Characterization of Organic Compounds

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All the solvents and reagents were chemical grade obtained from commercial suppliers and employed without further purification. Progress of the reactions were monitored by TLC (thin-layer chromatography) on aluminum-backed sheets with silica gel 60 GF254 (HX805651) and a fluorescent indicator (visualized with UV light of 254 nm). Flash chromatography was performed using silica gel 60 (230–400 mesh) for further purification of the products obtained. Melting points (mp) were determined on an Electrothermal IA 91,000 apparatus (Electrothermal, Bibby Scientific, Staffordshire, ST15 OSA, UK), and are reported as uncorrected. IR spectroscopy was obtained on a Perkin-Elmer 16 FPC FT infrared spectrophotometer and only significant absorption bands are reported as wavenumbers (cm-1) for the representative chemical groups. 1H and 13C NMR spectra were obtained on a Varian Mercury 300 MHz spectrometer or a Bruker Avance III 750 MHz spectrometer using deuterated chloroform (CDCl3) as the solvent and TMS as the internal standard. Chemical shifts (δ) are reported in ppm downfield from the internal standard and coupling constants are reported in Hertz (Hz) (supplementary material). Electrospray ionization high resolution mass spectrometry positive mode (ESI-HRMS) was performed with an Agilent 6545 QTOF LC/MS instrument (Agilent Technologies, Santa Clara CA, United States).
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3

Analytical Techniques for Compound Characterization

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Melting points were determined on a Gallenkamp (UK) apparatus and are uncorrected. All NMR spectra were obtained on either a Varian 300 MHz Mercury Spectrometer or Bruker 600 MHz Spectrometer. The TopSpin 3.5 software running on the Bruker NMR has a multiplet analysis tool (MANA) that identifies and defines multiplets automatically or interactively. Elemental analyses were carried out by Atlantic Microlab, Inc., Norcross, GA, and are within 0.4% of theory unless otherwise noted. Flash chromatography was performed on Isolera I (Biotage) instrument on silica gel (Davisil grade 634) with gradient elution varying from 100% Hexane to 100% EtOAc as a standard procedure except where otherwise indicated. Starting materials were obtained from Sigma–Aldrich and were used without further purification. Yields reported in the manuscript are not optimized yields.
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4

Characterization of Organic Compounds

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Melting points were determined on a Gallenkamp (UK) apparatus and are uncorrected. All NMR spectra were obtained on either a Varian 300 MHz Mercury Spectrometer or 600 MHz Bruker Spectrometer. Elemental analyses were carried out by Atlantic Microlab, Inc., Norcross, GA, and are within 0.4% of theory unless otherwise noted. Flash chromatography was performed with Davisil grade 634 silica gel. Starting materials were obtained from Sigma–Aldrich and were used without further purification.
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5

Melting Point and NMR Analysis Protocol

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Gallenkamp (U.K.) apparatus
was used to determine melting points and is uncorrected. All NMR spectra
were obtained either on a Varian 300 MHz Mercury Spectrometer or 600
MHz Bruker Avance Spectrometer, and the free induction decay (FID)
data were processed using Mestrelab’s Mnova NMR software (version
8.1) to obtain the reported NMR data. Elemental analyses were carried
out by Atlantic Microlab, Inc., Norcross, GA, and are within 0.4%
of theory unless otherwise noted. Flash chromatography was performed
using a Biotage Isolera flash chromatographic system with Davisil
grade 634 silica gel. Starting materials were obtained from Sigma-Aldrich
and were used without further purification. All microwave-assisted
syntheses (MWASs) were carried out using a Biotage Initiator. 1H and 13C NMR data were obtained for all the intermediates
and were consistent with our previously reported NMR spectral data.17 (link)1H and 13C NMR data were
obtained for SYA0340 free base as reported here.
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