The NMR experiments were carried out in a Bruker Avance III spectrometer using a 14.1 Tesla, (600.12 MHz in hydrogen frequency) magnetic field and 3 mm inverse triple cryoprobe 1H, 13C, and 15N nuclei. Each fraction was solubilized using 180 µL of CD3CN (Sigma-Aldrich Co., Darmstadt, Germany). Chemical shifts to all experiments were calibrated from the solvent signal (CD3CN) at 1.94 ppm. 1H experiments were performed using the zg30 pulse sequence. Instrumental parameters were set up as follow: 1.0 s relaxation delay, spectral width from 0 to 12 ppm, 32 k points, and 2.72 s of acquisition time. The post-processing was performed using a 0.1 Hz (Line Broadening—LB) exponential multiplication factor, and phase and baseline were manually corrected. 1H-13C HMBC experiments (hmbcetgpl3nd) were carried out using a spectral width of 0 to 10 ppm for the F2 dimension (1H) and 0 to 200 ppm for the F1 dimension (13C). An acquisition time of 0.0852 s, relaxation delay 2 s, and 32 scans for 128 increments was employed. Mono dimensional 1H TOCSY (seldigpzs) experiments were performed at 7.18, 6.909, and 6.86 ppm. Regarding these experiments, the following conditions were used: spectral width of 0 to 10 ppm, 2.72 s acquisition time, 1.0 s relaxation delay, 32 k points, and 128 scans.
Cd3cn
Manufactured by Merck Group
Sourced in Germany, United States
CD3CN is a chemical compound used as a solvent in nuclear magnetic resonance (NMR) spectroscopy. It is a deuterated form of acetonitrile, with the hydrogen atoms replaced by deuterium atoms. CD3CN is commonly used as a solvent for analyzing samples in NMR experiments due to its chemical stability and compatibility with a wide range of organic compounds.
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Lab products found in correlation
Acetonitrile, by Thermo Fisher Scientific (2 mentions)
Cd3od, by Merck Group (2 mentions)
Avance 3, by Bruker (1 mentions)
Dichloromethane, by Thermo Fisher Scientific (1 mentions)
Toluene, by Thermo Fisher Scientific (1 mentions)
Silver tetrafluoroborate, by Merck Group (1 mentions)
Tetrabutylammonium hexafluorophosphate, by Merck Group (1 mentions)
Lithium chloride (licl), by Merck Group (1 mentions)
N n dimethylformamide (dmf), by Thermo Fisher Scientific (1 mentions)
Diethyl ether, by Thermo Fisher Scientific (1 mentions)
Triphenylphosphine, by Merck Group (1 mentions)
2 2 biquinoline, by Merck Group (1 mentions)
Cd3 2co, by Merck Group (1 mentions)
Pyridine, by Merck Group (1 mentions)
1 10 phenanthroline, by Merck Group (1 mentions)
Hp 5ms capillary column, by Agilent Technologies (1 mentions)
Isq qd mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Trace 1300, by Thermo Fisher Scientific (1 mentions)
Acetonitrile, by Merck Group (1 mentions)
Topspin, by Bruker (1 mentions)
6 protocols using cd3cn
1
NMR Characterization of Compound Fractions
2
Ruthenium Complex Synthesis and Characterization
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All materials were used as received without further purification, including 1,10-phenanthroline, 2,2′-biquinoline, CD3CN, CD3OD, (CD3)2CO, lithium chloride, pyridine, silver tetrafluoroborate, tetrabutylammonium hexafluorophosphate, and triphenylphosphine which were purchased from Sigma-Aldrich. Ethanol (200 proof) was obtained from Decon Laboratories, acetone, acetonitrile, dichloromethane, diethyl ether, N,N-dimethylformamide, 85% H3PO4, and toluene were acquired from Fischer Scientific, and ammonium hexafluorophosphate was purchased from Oakwood Chemical. Complexes 1b and 2b,41 (link) [Ru(phen)2Cl2],42 (link) [Ru(p-cymene)Cl2]2,43 (link) and triphenylphosphine oxide44 (link) were prepared according to literature procedures.
3
NMR Spectroscopy and GC-MS Analysis
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All 1H NMR spectra were reported in units of parts per million (ppm) and measured relative to the signals for residual chloroform (7.26 ppm) in CDCl3/and for residual CH3CN in CD3CN at 1.96 ppm, unless otherwise stated. All 13C NMR spectra were reported in ppm relative to CDCl3 (77.23 ppm), unless otherwise stated and were obtained with 1H decoupling. Acetonitrile, CD3CN, FeIICl2, FeIIBr2, and trimethylsilyltriflate (TMSOTf) were purchased from Sigma Aldrich. Diethyl ether was procured from Spectrochem chemicals. Ethylbenzene was bought from TCI. H218O was purchased from Sigma Aldrich and ICON-isotope. 2-(Chloromethyl)quinoline hydrochloride was purchased from TCI and di(2-pyridyl)ketone was purchased from Alfa Aesar. All the products were analyzed by GC-MS analysis. GC-MS was performed on a Thermo Scientific ISQ QD Mass Spectrometer attached with a Thermo Scientific TRACE 1300 gas chromatograph using an HP-5ms capillary column (30 m × 0.25 mm × 0.25 μm, J&W Scientific) with helium as the carrier gas. The product yields were calculated from GC traces by comparing with the area percentage of standard products.
4
NMR Spectroscopy Analysis of Compounds 1 and 2
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NMR spectra of compounds 1 and 2 were obtained from solutions (500 µL) in acetonitrile-d3 (CD3CN, 99.96 atom % D; Sigma-Aldrich, St. Louis, MO, USA) using 5 mm o.d. Wilmad tubes (Sigma-Aldrich, St. Louis, MO, USA). The spectra were acquired on an Avance AVII 600 MHz NMR spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany) equipped with a 5 mm CP-TCI triple resonance inverse cryoprobe with a Z-gradient coil. NMR assignments were obtained from the examination of 1H, DEPT135, 1-D SELTOCSY, COSY, TOCSY, g-HSQC, g-HMBC, HSQC-TOCSY, and NOESY NMR spectra. The data were processed using Bruker TOPSPIN (version 2.1 pl4 or version 3) software. Chemical shifts, determined at 25 °C, were reported relative to internal CHD2CN (1.96 ppm) and CD3CN (118.26 ppm).
5
Purification of Common Solvents
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CDCl3, CD3CN, and DMSO-d6 were purchased
from Aldrich. All other reagents were obtained from commercial sources
and were used without further purification unless indicated otherwise.
from Aldrich. All other reagents were obtained from commercial sources
and were used without further purification unless indicated otherwise.
6
Physicochemical Characterization of Compounds
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Physical measurements 1 H and 13 C NMR spectra were recorded on a Varian Advance 400 MHz spectrometer at room temperature {CDCl 3 (99.8%, CIL), CD 3 CN (>99.8%, Aldrich), or CD 3 OD (>99.8%, Aldrich)}. Luminescence was measured on a Cary Eclipse Fluorescence Spectrophotometer with λ ex = 488 nm: emission spectra were collected from λ em = 500-800 nm. Absorbance (200-600 nm) was measured on a VARIAN CARY 50 Probe UV-visible spectrophotometer. Mass-spectroscopic analysis was performed by the RSC Mass-Spectrometry Facility (Research School of Chemistry, Australian National University, Canberra), and the Campbell Microanalytical Laboratory (Chemistry Department, University of Otago) performed the microanalyses.
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