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7 protocols using agilent 6210 esi tof

1

Spectroscopic Characterization of Compounds

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Elemental analyses of carbon, hydrogen, nitrogen and sulfur were determined using a Heraeus vario EL elemental analyzer. IR spectra were measured as KBr pellets on a Shimadzu IR Affinity-1 spectrometer between 400 and 4000 cm−1 or a Thermo Scientific Nicolet iS10 ATR spectrometer. The NMR spectra were recorded on a JEOL 400 MHz spectrometer. ESI TOF mass spectra were measured with an Agilent 6210 ESI TOF (Agilent Technologies, Santa Clara, CA, USA). All MS results are given in the form: m/z, assignment. UV-vis spectra were recorded on a Specord 40 (Analytik Jena) spectrophotometer in the wavelength range 200–700 nm. Time-Resolved Laser Fluorescence (TRLFS) was performed at T < 20 K using a pulsed Nd:YAG (Spectra Physics) pumped dye laser system (Radiant Dyes Narrow Scan K). The detection was carried out with a spectrograph (Shamrock 303i) equipped with a polychromator with 300, 600 and 1200 lines/mm gratings and an ICCD camera system (Andor iStar). Common concentrations were applied for the spectroscopic studies. In some cases, they were limited by the low solubility of the compounds.
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2

Comprehensive Analytical Techniques for Chemical Characterization

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1H and {1H}13C NMR spectra were recorded on Bruker instruments in the solvents indicated and were referenced to residual solvent peaks or internal TMS. Where present, structural assignments were performed with the help of COSY (3JH,H), HMQC (1JC,H), and HMBC (2JC,H and 3 JC,H) spectra and NOE experiments. UV–vis spectra were recorded either on Cary 50, 60, or 100 (Varian, Palo Alto, CA, USA, now Agilent, Santa Clara, CA, USA) or Specord S300 UV-vis (Analytik Jena, Jena, Germany) spectrometers in 1 cm glass or quartz cells, in the solvents indicated. Fluorescence emission spectra were recorded on a Cary Eclipse spectrometer in 1 cm glass or quartz cells, in the solvent indicated. FT-IR spectra were recorded on an Alpha (Bruker, Billerica, MA, USA) instrument (diamond ATR). Mass spectrometry analyses were performed on a QStar Elite (AB Sciex, Framingham, MA, USA) Quadrupole-TOF, Agilent 6210 ESI-TOF (Agilent, Santa Clara, CA, USA), or Ionspec QFT-7 ESI-FTICR (Varian Inc., Lake Forest, CA, USA) mass spectrometer.
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3

Spectroscopic Analysis of Compounds

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1H Nuclear Magnetic Resonance (NMR) (400 MHz) and 13C NMR (100.6 MHz) spectra were recorded on Bruker DPX-400 using transcranial magnetic stimulation (TMS) as internal standard. All spectra were recorded in CD3OD. High-resolution electron spray ionization mass spectra (HR-ESIMS) was carried out on Agilent 6210 ESI-TOF (Agilent Technology) mass spectrometer. Thin layer chromatography (TLC) study was carried out on silica gel plates (Kieselgel 60 F254, Merck) using solvent systems n-BuOH/AcOH/H2O (4:1:1) and CHCl3/MeOH (9:1). The spots were visualized by spraying anysaldehyde/conc. H2SO4 reagent, followed by heating at 110°C. Chromatography (CC) was carried out with Diaion HP-20 (Supelco) and silica gel 60 (40-60 μm, Merck).
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4

Characterization of Organoboron Compounds

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Dried solvents and argon as protection gas were used. 11B, 13C, 19F, 29Si, and 77Se NMR spectra were recorded with a JEOL ECZ 400R or with a JEOL ECS 400 spectrometer (128.25, 100.51, 376.13, 79, and 76.24 MHz, respectively). Chemical shifts δ are reported in ppm relative to BF3OEt2 (11B), Me4Si (13C, 29Si), CFCl3 (19F), and Me2Se (77Se).
For ESI‐TOF mass spectra, the samples were measured from CH3CN, CH3CN/CH2Cl2, CH3OH, or CH3CN/CH3OH solutions with an Agilent 6210 ESI‐TOF, Agilent Technologies, Santa Clara, CA, USA. The solvent flow rate was adjusted to 4 μL min−1, spray voltage set to 4 kV, drying gas flow rate was set to 15 psi (1 bar; ESI‐TOF=electrospray ionization–time of flight). Non‐ionic compounds were analyzed with a HR‐EI‐MS (Autospec Premier, Waters Co., Milford, MA, USA) using 80 eV electron energy.
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5

Characterization of Polyethylene Glycol Amphiphiles

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The 1H and 13C NMR spectra were recorded on JEOL 400 MHz and JEOL 100.5 MHz spectrometers (Tokyo, Japan) respectively; the solvent residual peak was used for referencing. The chemical shift values are on a δ scale, and the coupling constant values (J) are in Hertz. The HRMS data were collected on a Waters (Micromass) LCT1 using the ESI-TOF MS technique and Agilent 6210 ESI-TOF, Agilent Technologies, Santa Clara, CA, USA. Infrared spectra (IR) were recorded on a Perkin-Elmer FT-IR model 9 spectrometer. Molecular weight analysis M¯w , M¯n and the Polydispersity Index (PDI) of polyethyleneglycol (PEG) unit containing amphiphiles was done using an Agilent GPC system equipped with an Agilent 1100 pump and a refractive index detector, using PLgel columns, with THF as an eluent at a flow rate of 1.0 mL min−1 using polystyrene standards.
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6

Synthesis and Characterization of Triazolium Salts

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The triazolium salts [HL1]I [70 (link),87 (link)], [HL2]I [68 (link)] and [HL3]I [32 (link)] were prepared as described previously in the literature. Commercially available chemicals were used as purchased, unless otherwise noted. The solvents used for synthesis and catalysis were dried and distilled under inert gas and degassed by common techniques prior to use, unless otherwise noticed. 1H- and 13C-NMR spectra were recorded on a Jeol ECS 400 or Jeol ECZ 400R spectrometer (Joel, Munich, Germany) using the chemical shift of the solvent as an internal standard. Multiplets are reported as follows: singlet (s), duplet (d), triplet (t) quartet (q), quintet (quint), and combinations thereof. Mass spectrometry was performed on an Agilent 6210 ESI-TOF (Agilent, Walbronn, Germany).
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7

Characterization of Fluorescent Compounds

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The chemicals used were all commercially available from Aldrich, Acros Organics, Invitrogen, and mivenion GmbH and did not require further purification. All solvents were distilled before usage or purchased dry and in p.a. quality. For preparative work only distilled water and Milli-Q water obtained from a Millipore system were used. Dry solvents were taken from a MB SPS 800 solvent system from MBraun.
Instruments 1 H and 13 C NMR spectra were recorded on a Jeol ECX-400 (400 MHz 1 H-NMR and 176 MHz 13 C-NMR) spectrometer or a BrukerBioSpin (700 MHz) instrument at room temperature, and chemical shift values (δ) are given in ppm relative to the internal standard MeOD-d4 1 H-NMR spectra (3.31 ppm), 13 C NMR spectra (49.0 ppm). MS ESI-ToF analyses were performed on an Agilent 6210 ESI-TOF, Agilent Technologies, Santa Clara, CA, USA. The fluorescence spectra were recorded on a Jasco FP-6500 spectrofluorometer. UV/Vis spectra were recorded on a Scinco S-3100 spectrometer. The cell-based assay was performed on a Tecan InfiniteM200 Pro microplate reader equipped with a gas control module. For microscopy we used a Leica SP8 confocal laser scanning microscope and LASAF software. The flow cytometric studies were performed with a FACS-Canto II flow cytometer (BD Biosciences).
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