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Avance 300 mhz spectrometer

Manufactured by Bruker
Sourced in United States, Germany, Switzerland, France

The Avance 300 MHz spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analytical applications. It operates at a radiofrequency of 300 MHz and is capable of performing various NMR spectroscopy experiments to analyze the structure and properties of chemical compounds.

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52 protocols using avance 300 mhz spectrometer

1

Characterization of Organic Compounds

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All the chemicals were obtained from Sigma-Aldrich chemical company (USA), Lancaster (USA) and S.D. Fine chem. Limited (Mumbai). All the glassware is of borosilicate grade. Melting points were determined in open capillaries and are uncorrected. The purity of the compounds was ascertained by thin-layer chromatography (TLC) on silica gel-G plate.
Fourier transform infrared (IR) spectra were taken in KBr on a Thermo Nicolet Nexus 670 spectrophotometer. 1 H nuclear magnetic resonance (NMR) spectra were recorded on AVANCE 300 MHz spectrophotometer in CDCl 3 with tetramethylsilane (TMS) as internal standard. 13 C NMR spectra were recorded on BRUKER AVANCE 300MHz spectrometer in CDCl 3 with TMS as an internal standard. The chemical shift values are in δppm. Mass spectra were recorded on Polaris Q apparatus (Thermo Electron) and the fragmentations were obtained by electronic impact (EI). The data are given as mass to charge ratio (m/z) and nominal masses were used for the calculation of molecular weights of the prepared products.
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2

Physicochemical Characterization of Compounds

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All commercial reactants and solvents with the highest purity were purchased from either Sigma-Aldrich (St. Louis, MS, USA) or Alfa Aesar (Karlsruhe, Germany) and used without further purification. The melting points were determined on a Fischer-Johns block (Fisher Scientific, Schwerte, Germany) and are uncorrected. Elemental analyses were determined by an AMZ-CHX elemental analyzer (PG, Gdańsk, Poland) and are within ±0.4% of the theoretical values. ¹H-NMR spectra were recorded on an Avance 300 MHz) spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany). Analytical thin layer chromatography was performed with 60F254 silica gel plates (Merck, Darmstadt, Germany) and visualized by UV irradiation (254 nm). The physicochemical characterization of compounds 7 and 18 was presented in [43 (link),44 (link)]. The structure of 4 was presented in our previous publication [45 (link)], however no physicochemical characterization data was reported.
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3

Solid-State NMR Spectroscopy of Samples

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Solid-state nuclear magnetic resonance (SSNMR) spectra were acquired on a Bruker Avance 300 MHz spectrometer, equipped with a 7.05 T wide bore magnet. The experiments were performed at room temperature using a standard 4-mm magic angle spinning (MAS) probe with MAS rates of 10 kHz. A rotor-synchronized Hahn-echo sequence was employed with a π/2 pulse of 2 μs and a recycle delay of 5 or 10 s. Chemical shifts are referenced relative to ultrapure Milli-Q water (shift: + 4.7 ppm).
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4

Synthesis and Characterization of Fluorescent Probe for HOCl Detection

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All solvents and chemicals were purchased from commercial suppliers and were used without further purification unless otherwise stated. Column chromatography was conducted on silica gel (200–300 mesh) and thin layer chromatography (TCL) was performed using silica gel 60 F254 (Qingdao Ocean Chemicals, Qingdao, China). 1H NMR and 13C NMR spectra were recorded on a Bruker Avance 300 MHz spectrometer. High resolution mass spectra (HRMS) were recorded on an Agilent 1290LC-6540 Accurate Mass Q-TOF by using electrospray ionization (ESI). Fluorescent spectra were measured by using TU-1901 (Beijing Purkinje General Instrument Co., Ltd.) and F-280 (Tianjin Gangdong Technology Co., Ltd.). The cytotoxicity assay measures the absorption wavelength at 490 nm by means of an enzyme labeling device (Synergy HT). Fluorescence imaging of HOCl in live HeLa cells was measured under an Olympus FV1000 confocal fluorescence microscope.
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5

Characterization of Organic Compounds

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Sigma, Riedel-de Haën, and Merck, what provide the all reagents used. The 1 H and 13 C NMR spectra were determined on a Bruker Avance 300 MHz Spectrometer (Germany) at 300 MHz and 75 MHz, respectively, in CDCl 3 using tetramethylsilane as the internal calibration standard. IR spectra were saved with a Vertex 80v FT-IR (Germany). Melting point measurements were made by Electrothermal 9100 Melting Point Apparatus (China). Kinetic measurements of all compounds were obtained with a GBC Cintra 20 model Ultraviolet-Visible (UV-VIS) Spectrophotometer (Australia).
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6

NMR Characterization of Organic Compounds

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1H and 13C NMR spectra were recorded at 298 K on an Avance 300 MHz spectrometer (300 and 75 MHz, respectively; Bruker BioSpin). 1H-1H correlation spectroscopy (COSY) and 1H-13C heteronuclear single quantum coherence (HSQC) were used to confirm 1H and 13C assignments. Signals are reported as chemical shift (δ in ppm) relative to (CD3)2SO (1H NMR: δ = 2.50 ppm; 13 C NMR: δ = 39.52 ppm). Coupling constants (J) are reported in Hz and can be found in the Supplementary Information.
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7

Synthesis and Characterization of Functional Polymers

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Materials. Acetonitrile and triethylamine (Aldrich) were dried in a solvent purification system (J. C. Meyer). 2-Ethyl-2-oxazoline (EtOx; Aldrich) was distilled over barium oxide and stored under argon. Methyl tosylate (MeOTs) was distilled and stored under argon. Piperazine was purified by sublimation and stored under argon. (1R,8S,9s)-bicyclo[6.1.0]non-4-yn-9-ylmethyl (4-nitrophenyl) carbonate (BCN-PNP) was purchased from SynAffix and stored at -20°C. All other chemicals were purchased from Sigma-Aldrich or Acros Organics and used as received.
Instrumentation. Polymerizations were performed in a capped vial in a microwave reactor (Biotage Initiator Sixty) equipped with an IR temperature sensor. 1 H NMR spectra were recorded in CDCl 3 on a Bruker Avance 300 MHz spectrometer. Size-exclusion chromatography (SEC) was performed on a Agilent 1260-series HPLC system equipped with a 1260 online degasser, a 1260 ISO-pump, a 1260 automatic liquid sampler (ALS), a thermostatted column compartment (TCC) at 50°C equipped with two PLgel 5 µm mixed-D columns and a precolumn in series, a 1260 diode array detector (DAD) and a 1260 refractive index detector (RID) using N,Ndimethylacetamide containing 50 mM of LiCl (flow rate of 0.59 mL min -1 ) as solvent. Molar masses were calculated against polymethylmethacrylate standards.
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8

NMR Spectroscopy of PGT-Hormone Complexation

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Nuclear magnetic resonance spectra were obtained using an AVANCE 300 MHz spectrometer (Bruker). The samples (PGT and the IC in a 1:1 molar ratio) were dissolved in deuterated chloroform (CDCl3) at 25 °C. A chemical shift (δ) of 7.26 ppm for CDCl3 was used as internal reference.
The variation of chemical shift (Δδ) of the protons in the PGT due to the inclusion of the hormone into the cavity of the CD was calculated applying the following equation: Δδ=δIC-δFree where δIC is the proton shift of the PGT in the IC and δFree is the proton shift of the PGT when it is free i.e. not included.
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9

Characterization of Novel Organic Compounds

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General methods. All purchased chemicals were of the highest purity commercially available and used without further purification. Analytical grade solvents were used as received. Unless otherwise noted, all reactions were carried out under a nitrogen atmosphere. They were monitored by TLC on silica gel Alugram® Xtra SIL G/UV254. Column chromatography was performed on Machery-Nagel silica gel or neutral alumina.
NMR, mass and infrared spectra were obtained in the relevant 'Services communs de l'Institut de Chimie de Toulouse, Université de Toulouse III Paul-Sabatier'. 1 H-and 13 C-NMR spectra were recorded on a Bruker Avance 300 MHz spectrometer. Attributions of the signals were made using 2D NMR data (COSY, HSQC and HMBC). Protons and carbon atoms were numbered according to Fig. S25 †. Signals are described as follow: s, singlet; d, doublet; t, triplet; m, multiplet. App = Apparent; * = The multiplicity of the signal is more complex as it is part of an AAXX system. All spectra are given in Fig. were not possible with this apparatus. Fluorescence microscopy was performed with a Leitz Laborlux D fluorescence microscope equipped with an Andor Luca camera.
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10

Characterization of Wax Compounds by 13C-NMR

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13C-NMR spectra in solution were recorded on a Bruker Avance 300-MHz spectrometer (Rheinstetten, Germany) (75.48 MHz for 13C) at 373 K with D1 = 2 s. The samples were prepared by introducing 25 mg of the wax in 0.5 mL of 1,1,2,2-tetrachloro-1,2-dideuterioethane (C2D2Cl4) into a tube (5 mm outer diameter). The chemical shifts refer to the central peak of C2D2Cl4 used as internal reference at ∂ = 74.26 ppm.
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