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Arx 250

Manufactured by Bruker
Sourced in United States

The ARX-250 is a high-performance nuclear magnetic resonance (NMR) spectrometer produced by Bruker. It operates at a frequency of 250 MHz and is designed for a variety of analytical applications in chemistry, biochemistry, and materials science.

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3 protocols using arx 250

1

Characterization of Organic Compounds

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All solvents and chemicals were purchased from SDS and Aldrich, respectively. DMF, MeOH and CH3CN were dried using standard. 1H NMR and 13C NMR spectra were recorded on Bruker ARX-250 and Bruker Avance-500 spectrometers, respectively, and chemical shifts were reported in ppm downfield from TMS. IR spectra were obtained with a Perkin-Elmer Spectrum One FT-IR spectrometer equivuipped with a MIRacleTM single reflection horizontal ATR unit (germanium crystal). Electrospray ionization (ESI) mass spectrometry analyses and HRMS were obtained using Thermo Finnigan LCQ Advantage spectrometer. The elemental analyses were carried out by the mass spectrometry and microanalysis services in Gif-sur-Yvette (CNRS).
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2

Analytical Techniques for Organic Synthesis

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Analyses by thin layer chromatography (TLC) were performed on a Merck silica-gel 60 F254 (Darmstadt, Germany), and TLC plaques were visualized by UV-lamp at wavelengths of 254 and 365 nm. Unless otherwise noted, for column chromatography Merck silica-gel 60 (40–63 μm or 63–200 μm) was used. For gel-permeation or size-exclusion column chromatography Bio-Beads S-X1 from Bio-Rad Laboratories (Richmond, CA, USA) were used in toluene.
The NMR spectra were recorded on Bruker spectrometers: Avance-300, ARX-250 and Avance 500 (Billerica, MA, USA) at the Laboratoire de Chimie de Coordination, Toulouse, France. UV-visible spectra were obtained using a Perkin Elmer Lambda 25 (Waltham, MA, USA) or on a Varian Cary 100 Bio (Palo Alto, CA, USA) spectrophotometer in dichloromethane. Fluorescence spectra were recorded on a Perkin Elmer LS 55 spectrometer in dichloromethane at the Laboratoire de Chimie de Coordination in Toulouse, France. Elemental analyses were carried out by the Service de microanalyse at the Laboratoire de Chimie de Coordination in Toulouse, France.
The syntheses of monomer 8 and dimer 5 are summarized in Scheme 1 and Scheme 2 and described in the following sections.
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3

Determination of Degree of Branching by 1H-NMR

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Example 6

In order to determine the degree of branching by means of 1H-NMR spectroscopy, the samples were dissolved in D20 with 1% NaOH and measured at 70° C. In order to determine the degree of branching, the signals were required at 5.6 ppm (1) and 5.3 ppm (2) (solvent D20). Integration occurred via a previous base-line correction. The ratio in percent was calculated as follows:
[integral(2)*100]/[integral(1)+(2)]

The measurements were taken using a Bruker ARX 250 (Bruker ARX 250, 250 MHz 1H-NMR, solvent D20, 70° C.).

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