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¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are slanted or...
¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

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

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.
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...
Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)01:15

Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)

Insensitive Nuclei Enhanced by Polarization Transfer (INEPT) is an advanced Nuclear Magnetic Resonance (NMR) technique specifically designed to detect and enhance the signals of low-abundance nuclei, such as carbon-13 and nitrogen-15, in small molecules. The fundamental principle behind INEPT is the transfer of polarization from a more abundant and highly polarizable nucleus, typically hydrogen-1, to the low-abundance nucleus of interest. This process effectively boosts the NMR signal of the...
Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
Spin decoupling is usually achieved by...
2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other axis.

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Video Experimental Relacionado

Updated: Jul 5, 2026

NMR-Based Fragment Screening in a Minimum Sample but Maximum Automation Mode
09:19

NMR-Based Fragment Screening in a Minimum Sample but Maximum Automation Mode

Published on: June 4, 2021

Cribado basado en RMN de alto rendimiento con experimentos vinculantes de competencia.

Claudio Dalvit1, Maria Flocco, Stefan Knapp

  • 1Chemistry Department, Pharmacia, Viale Pasteur 10, 20014 Nerviano (MI), Milan, Italy. claudio.dalvit@pharmacia.com

Journal of the American Chemical Society
|June 27, 2002
PubMed
Resumen
Este resumen es generado por máquina.

Este estudio introduce un nuevo método de espectroscopia de RMN para el cribado de alto rendimiento, superando las limitaciones en la detección de ligandos de alta afinidad y covalentes. La técnica mejora la diversidad de compuestos y permite la detección rápida de miles de moléculas.

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Last Updated: Jul 5, 2026

NMR-Based Fragment Screening in a Minimum Sample but Maximum Automation Mode
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NMR-Based Fragment Screening in a Minimum Sample but Maximum Automation Mode

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Área de la Ciencia:

  • La bioquímica es la bioquímica.
  • Biología Química Biología química.
  • Biología Estructural Biología estructural.

Sus antecedentes:

  • El cribado de RMN basado en ligandos lucha con moléculas de alta afinidad y enlace covalente.
  • El rango de detección limitado restringe la diversidad de compuestos examinados mediante RMN.

Objetivo del estudio:

  • Desarrollar un nuevo enfoque de espectroscopia de RMN para el cribado de alto rendimiento.
  • Para superar las limitaciones de los métodos de detección de RMN existentes para la detección de ligandos y moléculas.
  • Para ampliar la gama de compuestos susceptibles a la detección de RMN, incluidos los de baja solubilidad.

Principales métodos:

  • Utiliza parámetros de relajación transversal y/o longitudinal selectivo.
  • Incorpora experimentos vinculantes para la competencia.
  • Deriva expresiones matemáticas para la configuración del experimento y la aproximación de constantes vinculantes.

Principales resultados:

  • Desarrolló con éxito una nueva metodología de detección de RMN.
  • Supera las limitaciones en la detección de ligandos de alta afinidad y enlaces covalentes.
  • Permite la detección de compuestos ligeramente solubles, aumentando la diversidad de compuestos seleccionados.
  • Permite la detección rápida de miles de compuestos contra objetivos biológicos.
  • Demuestra aplicabilidad para el cribado de extractos de plantas y hongos.

Conclusiones:

  • El nuevo método de detección de RMN avanza significativamente las capacidades de detección de alto rendimiento.
  • Esta técnica amplía el alcance del descubrimiento de fármacos basado en RMN y la detección de productos naturales.
  • El enfoque ofrece una plataforma más completa y eficiente para identificar nuevos ligandos y compuestos bioactivos.