Optical rotations were measured on JASCO P 1010 polarimeter; UV and FT-IR spectra were obtained by employing Hewlett Packard 8452A and Nicolet 510 instruments, respectively. All NMR spectra were recorded on a Bruker Avance DPX400 spectrometer. Spectra were referenced to the residual solvent signal with resonances at δH/C 7.26/77.1 (CDCl3). ESI MS data were acquired on a Waters Micromass LCT Classic mass spectrometer and Varian 500-MS LC Ion Trap. HPLC separations were performed using Waters 510 HPLC pumps, a Waters 717 plus autosampler, and Waters 996 photodiode array detector. All solvents were purchased as HPLC grade.
500 ms lc ion trap
Manufactured by Agilent Technologies
Sourced in United States
The 500-MS LC Ion Trap is a high-performance liquid chromatography-mass spectrometry (LC-MS) system designed for analytical applications. It features a robust and reliable ion trap mass analyzer capable of performing sensitive and accurate mass analysis. The instrument is engineered to provide consistent and reproducible results for a wide range of analytes.
Automatically generated - may contain errors
Lab products found in correlation
996 photodiode array detector, by Waters Corporation (1 mentions)
Avance dpx 400 spectrometer, by Bruker (1 mentions)
717 plus autosampler, by Waters Corporation (1 mentions)
Arx 600 mhz, by Bruker (1 mentions)
Nicolet nexus ftir, by Thermo Fisher Scientific (1 mentions)
Vario micro cube elemental analyzer, by Elementar (1 mentions)
Avance 3, by Agilent Technologies (1 mentions)
Ultrashield 400 plus, by Bruker (1 mentions)
8400s ft ir spectrophotometer, by Shimadzu (1 mentions)
Avance 3 600 mhz spectrometer, by Bruker (1 mentions)
Isopropyl alcohol, by Merck Group (1 mentions)
Vario el 3, by Elementar (1 mentions)
Aviii spectrometer, by Bruker (1 mentions)
Avance 3, by Bruker (1 mentions)
Spectramax gemini em, by Molecular Devices (1 mentions)
Galen 3 hot stage apparatus, by Leica (1 mentions)
Lambda 35 spectrophotometer, by PerkinElmer (1 mentions)
6 protocols using 500 ms lc ion trap
1
Spectroscopic Analysis of Organic Compounds
2
Synthesis and Characterization of Compound 2
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All reagents and solvents were purchased from Sigma-Aldrich and used without further purification. Compound 2 was prepared as described in [22 (link)]. Column chromatography was carried out on silica gel 60 (0.040–0.063 mm, 230–400 mesh, Fluka). 1H and 13C NMR spectra were recorded at room temperature (291 K) in CDCl3 on a Bruker ARX 600 MHz (600 MHz for 1H and 151 MHz for 13C). Chemical shifts are in ppm and coupling constants in Hz. Fourier transform-infrared (FT-IR) spectroscopy data were obtained from Thermo Nicolet Nexus FT-IR. The spectra were recorded from an accumulation of 32 scans in the range of 4000~400 cm−1. Mass spectra were recorded on Varian 500-MS LC Ion Trap. Elemental analyses were performed in the Microanalytical Laboratory of the Faculty of Chemistry, University of Lodz.
3
Spectroscopic Characterization of Organic Compounds
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IR spectra were recorded using a NICOLET iS50 instrument equipped with a liquid N2-cooled mercury-cadmium-telluride (MCT-A) detector. A flat crystal plate Zn-Se ATR unit (crystal thickness 4 mm) was used. The incidence angle was 45°. The ATR accessory was obtained from Pike Technologies.
1H NMR, 13C NMR, and 31P{H}NMR spectra were recorded on BRUKER Ultra Shield 400 Plus (400 MHz), BRUKER Avance III (600 MHz), and Varian Gemini (200 MHz) spectrometers, unless otherwise noted. Measurements were made in CDCl3 or DMSO-d6 solutions. Coupling constants were expressed in Hertz (Hz). 31P NMR spectra were obtained with the use of broadband 1H decoupling. Copies of IR and NMR spectra are presented atSupplementary Materials Figures S1–S54 . Electrospray ionization mass spectra were performed on a Varian 500-MS LC ion trap (University of Lodz). Elemental analysis was performed on a Micro Vario Cube elemental analyzer (Elementar).
1H NMR, 13C NMR, and 31P{H}NMR spectra were recorded on BRUKER Ultra Shield 400 Plus (400 MHz), BRUKER Avance III (600 MHz), and Varian Gemini (200 MHz) spectrometers, unless otherwise noted. Measurements were made in CDCl3 or DMSO-d6 solutions. Coupling constants were expressed in Hertz (Hz). 31P NMR spectra were obtained with the use of broadband 1H decoupling. Copies of IR and NMR spectra are presented at
4
Synthesis and Bioactivity of Ruthenium(II) Complexes
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All starting reagents: [RuCl2(p-cymene)2]2 dimer, anhydrous solvents: dichloromethane, isopropyl alcohol, diethyl ether were purchased from Sigma-Aldrich and Avantor Performance and they were commercially available. Synthesis of complexes was carried out in the argon atmosphere conditions using Schlenk techniques. Ligands 1a, 1c and 1d were prepared with the use of methods described before.20,23,24 (link) The 1H NMR and 13C NMR spectra were registered in DMSO-d6 (for all complexes) and CDCl3-d (for ligand 1b) using Bruker Avance III 600 MHz spectrometer. The IR spectra were recorded in KBr on the FTIR-8400S Shimadzu Spectrophotometer. The ESI-MS spectra were measured on Varian 500-MS LC Ion Trap. An elemental analysis was performed at the Faculty of Chemistry (University of Lodz) using a Vario Micro Cube by Elemental analyzer. Melting points of all compounds were determined in open capillary tubes on Büchii apparatus B-540 and were uncorrected. Anticancer activity was tested against three cancer cell lines: HL-60, NALM-6 and WM-115 in the Department of Bioorganic Chemistry at the Medical University of Lodz (anticancer), while antimicrobial activity was carried out on selected bacteria and fungi strains were done in the Department of Immunology and Infectious Biology at the University of Lodz. The MTT method was used to determine cells viability.
5
Synthesis and Characterization of α-Hydroxyiminoketones
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Commercial chemicals and solvents were used as received. If not stated otherwise, products were purified by filtration through a short silica gel plug (200–400 mesh) by using freshly distilled solvents as eluents or by recrystallization. Melting points were determined in capillaries with an Aldrich Melt-Temp II, and they are uncorrected. NMR spectra were taken with a Bruker AVIII spectrometer (1H NMR (600 MHz), 13C NMR (151 MHz), and 19F NMR (565 MHz); chemical shifts are relative to the residual undeuterated solvent peaks (CDCl3: 1H NMR δ = 7.26, 13C NMR δ = 77.16 [34 (link)]) or to the external standard (CFCl3: 19F NMR δ = 0.00). IR spectra were measured with an Agilent Cary 630 FTIR spectrometer neat. Mass spectra (ESI) were obtained with a Varian 500-MS LC Ion Trap. Elemental analyses were obtained with a Vario EL III (Elementar Analysensysteme GmbH) instrument. Starting α-hydroxyiminoketones 5a [35 (link)] and 5b [36 (link)] were prepared following the general literature protocols.
6
Analytical Characterization of Target Compounds
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Analytical grade reagents were purchased and used as supplied. Solvents were dried according to standard methods [1] . The chemical reactions were monitored by TLC using alumina plates coated with silica gel 60 F254 (Merck). Column chromatography separations were performed on silica gel Merck 230-400 mesh (Geduran Si 60). The melting points (m.p.) were measured with a Leica Galen III hot stage apparatus and are uncorrected. The 1 H-and 13 C-NMR spectra were recorded on Bruker AVANCE III spectrometers at 300 and 400 MHz, respectively. Chemical shifts (δ) are reported in ppm from the standard internal reference tetramethylsilane (TMS). The following abbreviations are used: s = singlet, d = doublet, t = triplet, m = multiplet. Mass spectra (ESI-MS) were performed on a 500 MS LC Ion Trap (Varian Inc., Palo Alto, CA, USA) mass spectrometer equipped with an ESI ion source, operated in the positive or negative ion mode. For the target compounds, the elemental analyses were performed on a Fisons EA1108 CHNS/O instrument at LAIST and were within the limit of ± 0.4%. The electronic spectra were recorded with a Perkin Elmer Lambda 35 spectrophotometer, using thermostated 1-cm path length cells and the fluorescence measurements were performed with a Spectramax Gemini EM (Molecular Devices) fluorimeter.
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