Ru complex 1 [19 ] and [Ru(bpy)3](PF6)3[23 ] were prepared according to previously reported procedures. High-resolution mass spectra measurements were recorded on a Bruker Daltonics microTOF spectrometer equipped with an electrospray ionization (ESI) source, and the experimental parameters were set to the following: Capillary temperature, 180 °C; capillary voltage, 4500 V; flow rate, 4.0 L min−1; capillary exit, 160 V; skimmer, 53.3 V; hexapole, 24 V.
Daltonics microtof spectrometer
Manufactured by Bruker
Sourced in Germany
The Daltonics microTOF spectrometer is a compact, high-performance time-of-flight mass spectrometer designed for precise mass determination. It utilizes a microfocusing reflectron technology to achieve high mass resolution and accuracy. The microTOF spectrometer is capable of analyzing a wide range of sample types, including small molecules, peptides, and proteins.
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Lab products found in correlation
Spectrum one spectrometer, by PerkinElmer (4 mentions)
Ultrashield spectrometer, by Bruker (2 mentions)
Avance 400, by Bruker (1 mentions)
Kieselgel 60, by Merck Group (1 mentions)
Avance 400 nmr spectrometer, by Bruker (1 mentions)
Avance 300 nmr, by Bruker (1 mentions)
P 1020 polarimeter, by Jasco (1 mentions)
7 protocols using daltonics microtof spectrometer
1
Mass Spectrometry of Ruthenium Complexes
2
Synthesis and Functionalization of 2-Bromo-benzo[c]phenanthrene
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Commercially available reagent grade materials such as 2-naphthaldehyde and 2,6-dimethoxy-4-bromobenzaldehyde were used as obtained. The synthesis of 2-bromo-benzo[c]phenanthrene as well as its subsequent functionalisation were carried out following methodology described in the literature12,13 (link) except for the photocyclisation steps which were adapted and are described below. THF was distilled from sodium/benzophenone ketyl. Column chromatography was performed with silica gel from Merck (Kieselgel 60; 63–200 μm or 40–63 μm). 1H NMR spectra were recorded on Bruker Avance 400 (400 MHz) or 500 (500 MHz) spectrometers. Chemical shifts are given in parts per million (ppm) by taking the solvent as a reference δCHCl3 = 7.26 ppm for 1H NMR and δCHCl3 = 77.16 ppm for 13C NMR. The coupling constants (J) are given in Hertz (Hz) and the multiplicity of the signals are expressed as: s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet. Mass spectrometry (MS and HRMS) experiments were performed on a Bruker Daltonics microTOF spectrometer (Bruker Daltonik GmbH, Bremen, Germany) by the Service de Spectrométrie de Masse de la Fédération de Chimie “Le Bel” (FR 2010). Irradiation of stilbene derivatives was carried out with a Heraeus TQ 150 mercury vapor lamp in a 400 mL photoreactor. The protons of 1H spectra were assigned according to Martin's proposed nomenclature.1a
3
Synthesis and Characterization of Compounds 6a-6g
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Compounds 6a–g were synthesized according to our previously reported method [44 (link)]. All chemicals were delivered and used without any further purification. 1H, 19F and 13C NMR spectra were recorded at 400 MHz, 377 MHz and 100 MHz, respectively. High-resolution mass spectra (HRMS) were recorded on a Bruker Daltonics microTOF spectrometer with an electrospray ionizer. FT-IR spectra were measured on a Perkin-Elmer Spectrum One spectrometer (KBr). Ultrasonication was done in a SY5200DH-T ultrasound cleaner. Melting points were measured by using the capillary tube method with an Electrothermal IA9100 apparatus (UK).
4
Ruthenium-catalyzed Organic Transformations
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All reactions and other manipulations were performed under nitrogen or argon atmosphere using standard Schlenk techniques. All reagents and solvents were obtained from commercial suppliers and used directly without further purification. The solvents were dried by standard techniques when needed. 1H and 13C NMR spectra were recorded using a Bruker UltraShield spectrometer at 500 or 400 and 101 MHz, respectively. Chemical shifts (δ) are reported in ppm using the residual solvent peak [[D6]DMSO (δ(H)=2.50 and (δ(C)=39.52 ppm); CDCl3 (δ(H)=7.26)] as an internal standard. Splitting patterns are denoted as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), dd (doublet of doublets), td (triplet of doublets), and br (broad). ESI‐HRMS was performed using a Bruker Daltonics microTOF spectrometer. IR spectra were recorded using a PerkinElmer Spectrum One spectrometer using solid samples prepared as KBr discs. Elemental analysis was performed by MEDAC Ltd (Chobham, Surrey, UK). [Ru(DMSO)4Cl2],15 [Ru(bpy)3](PF6)3,16 [Ru(bpy)3](PF6)2,17 and [Ru(bpy)2(deeb)](PF6)218 were synthesized according to literature methods.
5
NMR, IR, and HRESIMS Characterization Protocol
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1H- and 13C-NMR spectra were recorded in CDCl3 or DMSO-d6 using a Bruker AVANCE 300 NMR or a Bruker AVANCE 400 NMR spectrometer. 1H-NMR and 13C-NMR chemical shifts (δ) Chemical shifts were expressed in ppm and referenced to the residual solvent signals. Coupling constants (J) were reported in Hertz (Hz). IR spectra were recorded on a PerkinElmer Spectrum One Spectrometer using a universal attenuated reflectance (ATR) technique and are reported in cm-1. HRESIMS analysis was determined using a Bruker Daltonics microTOF spectrometer. Optical rotations were measured on a JASCO P-1020 polarimeter. All glassware was heat-dried prior to use. TLC were visualized using UV light (254 and 366 nm) and Godin’s reagent.
6
Mass Spectrometry Protocol for Analysis
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The mass spectra were recorded on a Bruker Daltonics micrOTOF spectrometer.
7
Characterization of Organic Compounds
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Chemical reagents in high purity were obtained commercially and were used without further purification. Melting points were determined in open capillaries using an Electrothermal IA9100 melting point apparatus (UK). 1H and 13C NMR spectra were recorded using a Bruker UltraShield spectrometer at 400 and 100 MHz, respectively. High resolution mass spectra (HRMS) were performed utilizing a Bruker Daltonics microTOF spectrometer. FT-IR spectra were obtained with potassium bromide pellets in the range of 400–4000 cm−1 using a Perkin-Elmer Spectrum One spectrometer. Ultrasonication was done in a SY5200DH-T ultrasound cleaner.
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