The 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded on a Bruker Avance spectrometer 400 at 400 MHz and 100 MHz, respectively. Chemical shifts are given in ppm (δ) referenced to CDCl3 with 7.26 for 1H and 77.10 for 13C, and to d6-DMSO with 2.50 for 1H and 39.5 for 13C. In the case of multiplet, signals are reported as intervals and abbreviated as follows: s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet. Coupling constants are expressed in hertz. High-resolution mass spectra (HRMS) were recorded on a BRUKER VPEXII spectrometer with ESI mode unless otherwise stated. Melting point was measured by BUCHI Melting Point B-540. The progress of the reactions was monitored by thin-layer chromatography on a glass plate coated with silica gel with fluorescent indicator (GF254). Column chromatography was performed on silica gel (200–300 mesh).
Vpexii spectrometer
Manufactured by Bruker
The VPEXII spectrometer is a versatile analytical instrument designed for high-performance electron paramagnetic resonance (EPR) spectroscopy. It offers precise magnetic field control and sensitive signal detection, enabling researchers to study the structure and dynamics of paramagnetic species in a wide range of materials and samples.
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5 protocols using vpexii spectrometer
1
NMR Spectroscopy Data Reporting Protocol
2
Synthetic Procedures for Organic Compounds
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Unless otherwise
noted, all reactions were carried out under air atmosphere, and commercial
materials and solvents were used without further purification. 1H NMR and 13C NMR spectra were measured on a 600
MHz spectrometer (1H NMR: 600 MHz, 13C NMR:
150 MHz) using CDCl3 or DMSO-d6 as the
solvent at room temperature. High-resolution mass spectra (HRMS) were
recorded on a BRUKER VPEXII spectrometer with ESI mode. Flash column
chromatography was performed on a silica gel, 200–300 mesh.
noted, all reactions were carried out under air atmosphere, and commercial
materials and solvents were used without further purification. 1H NMR and 13C NMR spectra were measured on a 600
MHz spectrometer (1H NMR: 600 MHz, 13C NMR:
150 MHz) using CDCl3 or DMSO-d6 as the
solvent at room temperature. High-resolution mass spectra (HRMS) were
recorded on a BRUKER VPEXII spectrometer with ESI mode. Flash column
chromatography was performed on a silica gel, 200–300 mesh.
3
Synthesis and Characterization of CDPIs
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All solvents were commercially available and were used without further purification unless stated. The chemicals used were either purchased from commercial sources or prepared according to literature procedures for CDPIs. The 1H, 13C nuclear magnetic resonance (NMR) spectra were recorded on a Bruker Avance spectrometer 400 at 400 MHz, 100 MHz respectively. Chemical shifts are given in ppm (δ) referenced to CDCl3 with 7.26 for 1H and 77.10 for 13C, and to d6-DMSO with 2.50 for 1H and 39.5 for 13C. In the case of multiplet, the signals are reported as intervals. Signals are abbreviated as follows: s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet. Coupling constants are expressed in hertz. Mass spectra were recorded on a BRUKER VPEXII spectrometer (ESI mode). The progress of the reactions was monitored by thin-layer chromatography on a glass plate coated with silica gel with fluorescent indicator (GF254). Column chromatography was performed on silica gel (200–300 mesh).
4
Spectroscopic Characterization of Organic Compounds
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NMR–spectra were recorded on Bruker AvanceIII–400M and AscendTM 500M in solvents as indicate. Chemical shifts (δ) are given in ppm relative to tetramethylsilane (δ = 0). The residual solvent signals were used as references and the chemical shifts converted to the TMS scale. The following abbreviations were used to describe peak splitting patterns: s (singlet), bs (broad singlet), d (doublet), t (triplet), q (quartet), m (multiplet), dd (doublet of doublets), dt (doublet of triplets). Coupling constants (J) were reported in hertz unit (Hz). High–resolution mass spectra (HRMS) were recorded on a Bruker VPEXII spectrometer with EI and ESI mode unless otherwise stated. Analytical thin layer chromatography was performed on Polygram SIL G/UV254 plates. Visualization was accomplished by UV light (254 nm), or KMnO4 staining solutions followed by heating, also by Gas chromatograph-Mass spectrometer analysis (GC-MS) on Agilent Technologies 5977A MSD. Flash column chromatography was performed using silica gel (200–300 mesh). Unless otherwise noted, all commercially available materials were used without further purification. All reactions were performed in glassware under argon. Anhydrous DCM, CH3CN, DMF and DMSO were purchased from Enery Organics and stored under argon.
5
Optimized Synthesis and Characterization of Organic Compounds
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Unless otherwise
noted, all reactions were carried out under the air atmosphere; commercial
materials and solvents were used without further purification. 1H NMR (400 MHz, 500 MHz, or 600 MHz) and 13C NMR
(101 MHz, 126 MHz, or 151 MHz) spectra were measured using CDCl3 or DMSO-d6 as the solvent at
room temperature. High-resolution mass spectra were recorded on a
Bruker VPEXII spectrometer with the ESI mode. Flash column chromatography
was performed on silica gel with 200–300 mesh.
noted, all reactions were carried out under the air atmosphere; commercial
materials and solvents were used without further purification. 1H NMR (400 MHz, 500 MHz, or 600 MHz) and 13C NMR
(101 MHz, 126 MHz, or 151 MHz) spectra were measured using CDCl3 or DMSO-d6 as the solvent at
room temperature. High-resolution mass spectra were recorded on a
Bruker VPEXII spectrometer with the ESI mode. Flash column chromatography
was performed on silica gel with 200–300 mesh.
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