Melting points were determined with a Reichert Thermopan apparatus. The 1H- and 13C-NMR spectra were recorded with a Bruker Avance 300 MHz and Varian 500 MHz spectrometer using TMS as the internal standard in DMSO-d6 or CDCl3. The IR spectra were recorded using a Perkin-Elmer Spectrum One Fourier Transform (FTIR) spectrophotometer. High-resolution mass spectral analyses were performed using the electrospray ionization (ESI) method on the Xevo G2 QTOf mass spectrometer. HPLC measurements were run on a Novapak C18 column (150 mm x 3.9 mm, 4 µm) with a mobile phase containing buffer (pH = 4), methanol, and acetonitrile in a ratio of 550:300:150 v/v/v. The flow rate was maintained at 1.0 mL/min with a column temperature of 35°C. UV detection occurred at λ = 256 nm. All reagents were used as purchased unless otherwise stated. Reactions were performed under a nitrogen atmosphere and the work-ups were done in a well-ventilated fuming hood.
Avance 300 mhz
Manufactured by Agilent Technologies
The Avance 300 MHz is a nuclear magnetic resonance (NMR) spectrometer manufactured by Agilent Technologies. It operates at a frequency of 300 MHz and is designed for a wide range of analytical applications in chemistry, materials science, and other related fields.
Automatically generated - may contain errors
Lab products found in correlation
500 mhz spectrometer, by Agilent Technologies (1 mentions)
Synapt g2 qtof, by Waters Corporation (1 mentions)
Unity inova 500 mhz, by Agilent Technologies (1 mentions)
Isco combiflash rf, by Teledyne (1 mentions)
Tlc silica gel 60 f254 plate, by Merck Group (1 mentions)
Unity inova 500 mhz nmr spectrometer, by Agilent Technologies (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
400 mhz spectrometer, by Bruker (1 mentions)
Ltq orbitrap xl mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Kieselgel 40, by Merck Group (1 mentions)
7 protocols using avance 300 mhz
1
Synthetic Characterization of Small Molecules
2
Spectroscopy and Chromatography Methods
3
Characterization of Organic Compounds
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All reagents were obtained commercially and used as received unless otherwise stated. Solvents were dried as per the standard procedures. Melting points were determined on the Reichert thermopan melting point apparatus. The 1H- and 13C-NMR spectra were recorded on the Bruker Avance 300 MHz and Varian 500 MHz spectrometers using TMS as the internal standard in DMSO-d6 and CDCl3. The FTIR spectra were recorded on a Perkin-Elmer Spectrum One Fourier transform FTIR spectrophotometer. High-resolution mass spectral analyses were performed using the electrospray ionization (ESI) method on the Xevo G2 QTOf mass spectrometer. HPLC analyses were carried out as described in the European Pharmacopoeia for ganciclovir related substances.
4
Melting Point and Chromatographic Analysis
5
Synthesis of Pyrene-based Compounds
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All chemicals were obtained from
conventional commercial sources and used without further purification
unless otherwise noted. The synthesis of compound 2-(Bpin)pyrene (6 ) was performed according to the literature.37 (link)−39 (link) The synthesis of compound 2-bromopyrene (7 ) was carried
out according to the literature.39 (link)−41 (link) 3,4-Dimethoxystyrene
(9 ) was synthesized according to the literature.42 (link),43 (link) The synthetic method of compounds 4 and 5 is shown in the Supporting Information . Thin layer chromatography was performed on Merck silica gel 60F254 glass-backed plates. Flash chromatography was carried out
with silica gel 60. Nuclear magnetic resonance (NMR) spectra were
recorded on a Varian AVANCE 300 MHz instrument with solvent indicated.
The 1H NMR and 13C NMR chemical shifts are reported
in parts per million relative to tetramethylsilane or the residual
solvent protons.
conventional commercial sources and used without further purification
unless otherwise noted. The synthesis of compound 2-(Bpin)pyrene (
out according to the literature.39 (link)−41 (link) 3,4-Dimethoxystyrene
(
with silica gel 60. Nuclear magnetic resonance (NMR) spectra were
recorded on a Varian AVANCE 300 MHz instrument with solvent indicated.
The 1H NMR and 13C NMR chemical shifts are reported
in parts per million relative to tetramethylsilane or the residual
solvent protons.
6
Melting Point and NMR Analysis
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Melting points were determined using the open capillary method and are uncorrected. 1H NMR and 13C NMR spectra were recorded on either a Brucker Avance 300 MHz or a Varian Inova 400 and 500 MHz FT spectrometer using TMS as an internal standard (chemical shift in δ values, J in Hz). High resolution mass spectra and electrospray ionization recorded on QSTAR XL High resolution mass spectrometer. All regents and solvents used are commercially available. Column chromatography was performed using silica gel (60–120 mesh).
7
Characterization of Organic Compounds
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Melting points were taken on a Gallenkamp melting point apparatus and are uncorrected. 1 H and 13 C NMR spectra were recorded on a Bruker Avance 300 MHz, a Varian 300 MHz, or a Bruker 400 MHz spectrometer. Splitting patterns are described as singlet (s), doublet (d), triplet (t), quartet (q), quintuplet (qt), and broad (br). Chromatographic separations were performed on silica gel (Kieselgel 40, 0.040-0.063 mm, Merck). Reactions and products mixtures were routinely monitored by thin-layer chromatography (TLC) on Merck 0.2 mm precoated silica (60 F254) aluminum sheets, with visualization by irradiation with a UV lamp. ESIMS and HRESIMS were carried out by a Thermo Finningan LCQ Deca XP Max ion-trap mass spectrometer equipped with Xcalibur software, and an LTQ Orbitrap XL mass spectrometer (Thermo FisherScientific, San Jose, CA, USA) operated in positive ion mode, respectively. The Orbitrap mass analyzer was calibrated according to the manufacturer's directions using a mixture of caffeine, methionine-arginine-phenylalanine-alanine-acetate (MRFA), and Ultramark 1621 in a solution of acetonitrile, methanol, and acetic acid. Data were collected and analyzed using the software provided by the manufacturer.
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