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Lc msd tof spectrometer

Manufactured by Agilent Technologies
Sourced in United States

The LC/MSD TOF spectrometer is a laboratory instrument used for the analysis of chemical compounds. It combines liquid chromatography (LC) with time-of-flight mass spectrometry (TOF-MS) to provide accurate mass measurements and high-resolution separation of complex mixtures.

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4 protocols using lc msd tof spectrometer

1

Potassium Iodate-Mediated Oxidative Synthesis

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Reagents: unless otherwise indicated, all solvents and organic reagents were obtained from commercially available sources and were used without further purification. Acetone was dried by a molecular sieve. Potassium iodate (99%, Innochem) was used in this oxidative reaction.
Instrument: The reaction process was monitored by thin-layer chromatography (TLC, Yantai Jiangyou Co.Ltd, Tsingdao, Shandong, China) with silica gel plates (thickness = 0.20 mm, GF254) under UV light and LC-MS (Waters Acquity UPLC/SQD, Waters Acquity UPLC/SQD, Milford, MA, USA). Mass spectra were obtained using a Waters Acquity UPLC-SQD mass spectrometer. High-resolution mass spectra (HRMS, Thermo Scientific Exactive. Plus, 81 Wyman Street, Waltham, MA, USA) were recorded on an Agilent Technologies LC/MSD TOF spectrometer. The 1H-NMR spectra were recorded on a Varian Mercury 400 or 500 MHz instrument, and 13C-NMR spectra were recorded at 400 or 500 MHz on a Varian Mercury using dimethyl sulfoxide-d6 (DMSO-d6), methanol-d4 (CD3OD), chloroform-d (CDCl3) as the solvents and tetramethylsilane (TMS) as an internal standard.
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2

Platinum Complex Synthesis and Characterization

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Solvents and reagents were purchased from Sigma-Aldrich
unless otherwise noted. K2PtCl4 was purchased
from J. and J. Materials (NJ). NMR spectra were recorded at Bard College
using a Varian NMR-400 MHz spectrometer (1H, 400 MHz; 13C, 100.6 MHz). Shifts are given in parts per million and
coupling constant J values in Hertz. Abbreviations
used: s = singlet; d = doublet; t = triplet; and m = multiplet. Electrospray
MS was performed at Vassar College using an Agilent LC/MSD-TOF spectrometer.
Samples were run in chloroform in negative mode.
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3

Spectroscopic Analysis of Diazoimides and Alkylidenepyrazolones

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Proton (1H), carbon (13C), and fluorine (19F) NMR spectra were recorded on a Bruker Avance HD III spectrometer (400 MHz for 1H NMR, 100 MHz for 13C NMR, and 376 MHz for 19F NMR) and calibrated using tetramethylsilane (TMS) as internal reference. High resolution mass spectra (HRMS) were obtained on an Agilent Technologies LC/MSD TOF spectrometer under electrospray ionization (ESI) conditions. The melting point of compounds was determined using a melting point instrument. Flash column chromatography was performed on silica gel (0.035–0.070 mm) using compressed air. X-ray single crystals were obtained on a Rigaku 002 Saturn 944 spectrometer. Thin layer chromatography (TLC) was carried out on 0.25 mm SDS silica gel coated glass plates (60F254). Eluted plates were visualized using a 254 nm UV lamp. Unless otherwise indicated, all reagents were commercially available and used without further purification. All solvents were distilled from the appropriate drying agents immediately before use. Diazoimides 1a1g were synthesized according to the reported procedures [10 (link),46 (link),47 (link)]. Alkylidenepyrazolones 2a2q were prepared according to literature procedures [48 (link),49 (link),50 (link)].
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4

Copper(II)-phenanthroline Complex Characterization

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All reactions were performed under aerobic conditions and all reagents and solvents were purchased from Sigma-Aldrich or Acros Organics. The reference copper(II)-phenanthroline complex [Cu(H 2 O)(1,10-phenanthroline) 2 ](NO 3 ) 2 was prepared following the procedure described by K. J. Catalan et al. 69 pBR322 plasmid DNA was purchased from Roche and calf thymus DNA was obtained from Sigma-Aldrich. 1 H, 13 C { 1 H} and heteronuclear { 1 H-13 C}-HSQC NMR spectra were recorded at room temperature with a Varian Unity 400 MHz spectrometer. Proton and carbon chemical shifts are expressed in parts per million ( ppm, δ scale) and are referenced to the peak of the solvent used. Infrared spectra (as KBr pellets) were recorded using a Nicolet-5700 FT-IR (in the range 4000-400 cm -1 ), and data are represented as the frequency of absorption (cm -1 ). Elemental analyses were performed by the Servei de Microanalisi, Serveis Cientificotècnics of the University of Barcelona. UV-Vis experiments were performed with a Varian Cary-100 spectrophotometer. The fluorescence measurements were carried out with a KONTRON SFM 25 spectrofluorometer. ESI mass spectroscopy was carried out using a LC/MSD-TOF Spectrometer from Agilent Technologies, equipped with an electrospray ionization (ESI) source at the Serveis Cientificotècnics of the University of Barcelona.
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