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Related Concept Videos

NMR Spectrometers: Overview01:20

NMR Spectrometers: Overview

NMR spectrometers consist of a strong magnet, a radiofrequency transmitter, and a detector attached to a computer console for recording spectra of samples containing NMR-active nuclei. In first-generation NMR instruments called continuous-wave spectrometers, the resonance frequencies of the nuclei are determined by frequency-sweep or field-sweep methods. The magnetic field strength is fixed and the rf signal is swept in the former, while the radiofrequency signal is fixed and the magnetic field...
¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

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

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...
¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

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...
¹H NMR: Pople Notation01:09

¹H NMR: Pople Notation

The Pople nomenclature system classifies spin systems based on the difference between their chemical shifts. Coupled spins are denoted by capital letters with subscripts indicating the number of equivalent nuclei. When the coupled nuclei have well-separated chemical shifts, they are assigned letters that are far apart in the alphabet, such as A and X. When the difference in chemical shifts is small, coupled nuclei are named using adjacent letters of the alphabet (AB, MN, or XY).
A proton...
NMR Spectroscopy of Aromatic Compounds01:14

NMR Spectroscopy of Aromatic Compounds

Aromatic compounds can be identified or analyzed using proton NMR and carbon‐13 NMR. Typically, aromatic hydrogens or hydrogens directly bonded to the aromatic rings are strongly deshielded by the aromatic ring current. Therefore, they absorb in the range of 6.5–8.0 ppm in proton NMR spectra. For instance, aromatic hydrogens directly bonded to the benzene ring absorb at 7.3 ppm. However, aromatic hydrogens of larger rings absorb farther upfield or downfield than the ideal range. Consider...
Proton (¹H) NMR: Chemical Shift01:07

Proton (¹H) NMR: Chemical Shift

Organic molecules primarily contain carbon and hydrogen atoms. While all the hydrogen isotopes are NMR-active, protium or hydrogen-1 is the most abundant. It has a significant energy separation between its nuclear spin states due to its large gyromagnetic ratio. As per Boltzmann's distribution, an increase in the energy separation implies a greater excess population of nuclei available for excitation, resulting in a strong NMR absorption signal.
Absorption signals of all the protium nuclei in a...

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Pure Shift Nuclear Magnetic Resonance: a New Tool for Plant Metabolomics
13:16

Pure Shift Nuclear Magnetic Resonance: a New Tool for Plant Metabolomics

Published on: July 31, 2021

"Pure by NMR"?

Timothy D W Claridge1, Stephen G Davies, Mario E C Polywka

  • 1Department of Chemistry, Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK.

Organic Letters
|November 4, 2008
PubMed
Summary
This summary is machine-generated.

This study introduces a straightforward method using nuclear magnetic resonance (NMR) spectroscopy to precisely measure diastereoisomeric ratios. The technique accurately quantifies mixtures with high precision, even for challenging samples.

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Area of Science:

  • Analytical Chemistry
  • Organic Chemistry
  • Spectroscopy

Background:

  • Determining diastereoisomeric ratios is crucial in organic chemistry for understanding reaction stereoselectivity and product purity.
  • Traditional methods for quantifying diastereoisomers can be complex and lack precision for high ratios.

Purpose of the Study:

  • To develop a simple and accurate protocol for determining high diastereoisomeric ratios using quantitative proton nuclear magnetic resonance ((1)H NMR) spectroscopy.
  • To establish a method capable of quantifying ratios up to 1000:1 (99.8% de).

Main Methods:

  • Integration of a carbon-13–proton ((13)C-(1)H) satellite peak within a parent proton ((1)H) NMR resonance.
  • Comparison of the satellite peak intensity to the minor diastereoisomer's signal in a quantitative (1)H NMR spectrum.

Main Results:

  • The developed protocol accurately determines diastereoisomeric ratios, achieving precision for ratios as high as 1000:1.
  • The method demonstrates high accuracy, quantifying samples with up to 99.8% diastereomeric excess (de).

Conclusions:

  • This nuclear magnetic resonance (NMR) based protocol offers a simple, accurate, and highly precise method for quantifying diastereoisomeric ratios.
  • The technique is particularly valuable for analyzing complex mixtures and ensuring high stereochemical purity in synthesized compounds.