2D Ultrafast HMBC: A Valuable Tool for Monitoring Organic Reactions

Herrera, Antonio; Fernández-Valle, Encarnación; Gutiérrez, Eduardo Gutiérrez; Martínez‐Álvarez, Roberto; Molero, Dolores; Pardo, Zulay D.; Sáez, Estéban

doi:10.1021/ol902532f

Cited by 32 publications

(37 citation statements)

References 17 publications

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“…4.8 min rate. The apparent unstable character of the intermediate appears similar to other intermediates described in a recent work . It probably explains why previous attempt to detect this intermediate by conventional NMR methods was unsuccessful …”

Section: Resultssupporting

confidence: 84%

“…The advent of UF‐NMR opens the way to new applications in chemistry, including the real‐time monitoring of short time scale phenomena . Recently, the application of TOCSY, HSQC and HMBC UF‐NMR experiments was reported for the mechanistic study of a specific organic reaction, making possible to detect different intermediate species . UF‐NMR is emerging as a potential technique to study mechanisms in organic reactions at natural abundance.…”

Section: Introductionmentioning

confidence: 99%

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Real‐time mechanistic monitoring of an acetal hydrolysis using ultrafast 2D NMR

Queiroz

Giraudeau

Santos

et al. 2012

Magnetic Reson in Chemistry

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Ultrafast (UF) 2D NMR makes it possible to obtain a 2D NMR spectrum in less than a second. Here, UF-HSQC experiments are used for the real-time mechanistic study of an acetal hydrolysis at ¹³C natural abundance, and it is possible to characterize the presence of the hemiacetal, an intermediate with a well-known short lifetime. The assignments are confirmed and rationalized by quantum calculations of ¹H and ¹³C NMR chemical shifts and natural bonding orbital analysis.

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Section: Resultssupporting

confidence: 84%

Section: Introductionmentioning

confidence: 99%

Real‐time mechanistic monitoring of an acetal hydrolysis using ultrafast 2D NMR

Queiroz

Giraudeau

Santos

et al. 2012

Magnetic Reson in Chemistry

View full text Add to dashboard Cite

show abstract

“…In several other applications, the sensitivity was not an issue, but a few scans (typically two or four) were accumulated for phase cycling purposes, when the gradient‐based coherence selection was not sufficient . In the reported applications, it was typically the case when a strong signal needed to be suppressed, such as the solvent signal in 1 H NMR or the signal from 1 H bound to 12 C in heteronuclear NMR.…”

Section: Multi‐scan Single‐shotmentioning

confidence: 99%

“…During the last 10 years, numerous publications have been devoted to the development or applications of UF 2D NMR, and its performance has been improved dramatically, leading to an efficient analytical tool capable of targeting applications that were out of reach of conventional 2D NMR . The most emblematic of these applications is the monitoring of fast chemical or biochemical processes or the coupling with hyphenated techniques such as chromatography or dynamic nuclear polarization . Also noticeable is the development of NMR acquisitions in inhomogeneous fields or the quantitative perspectives opened by UF 2D NMR …”

Section: Introductionmentioning

confidence: 99%

Fast hybrid multi‐dimensional NMR methods based on ultrafast 2D NMR

Akoka

Giraudeau

2015

Magnetic Reson in Chemistry

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Conventional multi-dimensional (nD) NMR experiments are characterized by inherent long acquisition durations, while ultrafast (UF) NMR makes it possible to reduce to a few hundreds of milliseconds the overall acquisition duration of a complete nD NMR dataset. Although extremely promising for a number of specific applications, the UF strategy suffers from significant limitations compared with its conventional counterpart. The main limitations concern the sensitivity, the resolution, and the accessible spectral width. However, when the targeted applications are compatible with an acquisition duration between a few seconds and a few minutes, hybrid UF techniques can be used to improve the performance of UF nD NMR while remaining faster than conventional acquisitions. Much better results in terms of signal-to-noise ratio can be achieved with the multi-scan single-shot approach or with interleaved acquisitions. Even more, for the same experimental duration, and in the case of homonuclear 2D NMR, the multi-scan single-shot approach has a much higher precision than conventional 2D NMR. Interleaved 2D NMR overcomes the drawbacks of single-scan UF NMR in terms of spectral width and provides spectra for which the quality is not significantly different from that obtained with conventional 2D NMR. Finally, high spectral qualities have been demonstrated from hybrid conventional/UF 3D approaches capable of recording a whole 3D spectrum in the time needed to record a conventional 2D spectrum. This mini-review aims at describing the principles, the recent advances and the latest applications of these hybrid techniques. Copyright © 2015 John Wiley & Sons, Ltd.

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“…Consequently, a long acquisition time is needed, which limits its practical applications. Recently, ultrafast (UF) sequences based on spatially encoded iMQCs have generated tremendous interest, and some important applications on liquid samples have been performed . Compared to the conventional iMQC method, which takes more than 10 min, this technique provides iMQC spectra within 1 min …”

Section: Introductionmentioning

confidence: 99%

Feasibility of Ultrafast High‐Resolution Spectroscopy in the Analysis of Molecular‐Mobility‐Restricted Samples in Deuterium‐Free Environments

Cai

Jin

Cui

2018

J Chinese Chemical Soc

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The feasibility of ultrafast high-resolution intermolecular multiple-quantum coherence (UF-iMQC) spectroscopy for the direct analysis of molecular-mobility-restricted samples that are not suitable for magic-angle spinning, such as a jelly, hand soap, and marrow, is presented. Most components could be directly detected in their original state within 1 min without the need for tedious sample preparation processes. When we use conventional liquid nuclear magnetic resonance (NMR) method to study these systems, the spectral information could not be retrieved owing to the intrinsic inhomogeneous magnetic fields caused by sample inhomogeneity. In addition, the possibility for UF-iMQC-based quantifications is shown. The examples presented in this paper demonstrate the potential of UF iMQC NMR for food safety inspection, for quality testing of daily-life supplies, or in assisting medical diagnosis.

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2D Ultrafast HMBC: A Valuable Tool for Monitoring Organic Reactions

Cited by 32 publications

References 17 publications

Real‐time mechanistic monitoring of an acetal hydrolysis using ultrafast 2D NMR

Real‐time mechanistic monitoring of an acetal hydrolysis using ultrafast 2D NMR

Fast hybrid multi‐dimensional NMR methods based on ultrafast 2D NMR

Feasibility of Ultrafast High‐Resolution Spectroscopy in the Analysis of Molecular‐Mobility‐Restricted Samples in Deuterium‐Free Environments

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