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Related Concept Videos

Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

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The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse....
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¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

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The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
A broadband decoupling technique is used to simplify these complex, sometimes overlapping, signals. Broadband decoupling relies on a...
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¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR

1.1K
The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
1.1K
¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)

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When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
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¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

868
At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
868
2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

212
Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
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Chemical Analysis of an Isotopically Labeled Molecule Using Two-Dimensional NMR Spectroscopy at 34 μT.

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|October 16, 2023
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Low-field nuclear magnetic resonance (NMR) can reveal detailed molecular structures using isotopically labeled compounds. Two-dimensional correlation spectroscopy (COSY) on 1-13C-ethanol at ultra-low fields successfully mapped J-coupling networks.

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Area of Science:

  • Analytical Chemistry
  • Spectroscopy
  • Organic Chemistry

Background:

  • Low-field nuclear magnetic resonance (NMR) spectroscopy offers limited chemical shift resolution, challenging chemical analysis.
  • Isotopically labeled molecules present a potential solution, but their application in 2D NMR techniques is underexplored.

Purpose of the Study:

  • To investigate the utility of 2D NMR, specifically correlation spectroscopy (COSY), for analyzing isotopically labeled molecules at ultra-low magnetic fields.
  • To demonstrate the feasibility of obtaining detailed spectral information from low-field NMR experiments.

Main Methods:

  • Experimental and simulated correlation spectroscopy (COSY) were performed on 1-13C-ethanol at an ultra-low field of 34.38 μT.
  • Analysis focused on the splitting of the 1H spectrum due to heteronuclear coupling and the resulting J-coupling networks.

Main Results:

  • The 1H spectrum of 1-13C-ethanol exhibited significant splitting due to heteronuclear coupling, breaking magnetic equivalence.
  • The 2D COSY spectrum clearly resolved spectral details, revealing J-coupling networks.
  • Homonuclear coupling cross-peaks were observed only when coupled 1H spins shared identical 13C spin states.

Conclusions:

  • Ultra-low field 2D NMR, even with moderate line widths, can effectively elucidate J-coupling networks in isotopically labeled molecules.
  • This technique enhances the analytical capabilities of low-field NMR spectroscopy for complex chemical analysis.