Oxidative Neutralization of Mustard‐Gas Simulants in an On‐Board Flow Device with In‐Line NMR Monitoring

Picard, Baptiste; Gouilleux, Boris; Lebleu, Thomas; Maddaluno, Jacques; Chataigner, Isabelle; Penhoat, Maël; Felpin, François‐Xavier; Giraudeau, Patrick; Legros, Julien

doi:10.1002/ange.201702744

Cited by 15 publications

(10 citation statements)

References 51 publications

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“…It was also shown to remain the most competitive pulse sequence for the detection of small molecule signals in flow conditions (up to 2.0 mL.min À1 ). to monitor the neutralization of mustard gas mimetics through a 263 portable flow chemistry setting [34]. Two solvent signals needed 264 to be suppressed, which was achieved thanks to a WET-180-265 NOESY pulse sequence combined with a Sat block (Fig.…”

Section: Introductionmentioning

confidence: 99%

“…Thanks to this pulse sequence, the CEESO peak at 3.8 ppm can be efficiently detected through the flow reaction even at high flow-rate. Readers are referred to Ref [34]. for detailed peak assignments.…”

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confidence: 99%

“…C) Autonomous self-optimizable flow reactor used for the optimization of the derivative 8 and relying on benchtop NMR as an inline detector. Red dashed lines put into relief units under the control of the algorithm.Figures A, Breproduced with permission from[34];Figure Creproduced with permission from[35]. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)Fig.…”

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confidence: 99%

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Gradient-based pulse sequences for benchtop NMR spectroscopy

Gouilleux

Farjon

Giraudeau

2020

Journal of Magnetic Resonance

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Benchtop NMR spectroscopy has been on the rise for the last decade, by bringing high-resolution NMR in 30 environments that are not easily compatible with high-field NMR. Benchtop spectrometers are accessible, 31 low cost and show an impressive performance in terms of sensitivity with respect to the relatively low 32 associated magnetic field (40-100 MHz). However, their application is limited by the strong and ubiqui-33 tous peak overlaps arising from the complex mixtures which are often targeted, often characterized by a 34 great diversity of concentrations and by strong signals from non-deuterated solvents. Such limitations 35 can be addressed by pulse sequences making clever use of magnetic field gradient pulses, capable of per-36 forming efficient coherence selection or encoding chemical shift or diffusion information. Gradients 37 pulses are well-known ingredients of high-field pulse sequence recipes, but were only recently made 38 available on benchtop spectrometers, thanks to the introduction of gradient coils in 2015. This article 39 reviews the recent methodological advances making use of gradient pulses on benchtop spectrometers 40 and the applications stemming from these developments. Particular focus is made on solvent suppression 41 schemes, diffusion-encoded, and spatially-encoded experiments, while discussing both methodological 42 advances and subsequent applications. We eventually discuss the exciting development and application 43 perspectives that result from such advances.

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Gradient-based pulse sequences for benchtop NMR spectroscopy

Gouilleux

Farjon

Giraudeau

2020

Journal of Magnetic Resonance

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“…It was through specifically designed Halbach arrays of magnets [15], advancements in shimming electronics, and temperature stabilisation that these tens-of-ppb magnetic field homogeneities were achieved [16][17][18]. From this point, a range of high-resolution benchtop NMR spectrometers with different field strengths and heteronuclear detection capabilities have been developed and implemented across a plethora of applications [19], such as industrial quality control [20][21][22][23][24][25][26], 1 H and 13 C NMR undergraduate teaching [27][28][29][30][31][32], and on-line reaction monitoring [33][34][35][36][37][38][39].…”

Section: Introductionmentioning

confidence: 99%

Hyperpolarised 1H–13C Benchtop NMR Spectroscopy

Robinson¹,

Richardson²,

Halse³

2019

Applied Sciences

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Benchtop NMR spectrometers with sub-ppm spectral resolution have opened up new opportunities for performing NMR outside of the standard laboratory environment. However, the relatively weak magnetic fields of these devices (1–2 T) results in low sensitivity and significant peak overlap in 1H NMR spectra. Here, we use hyperpolarised 13C{1H} NMR to overcome these challenges. Specifically, we demonstrate the use of the signal amplification by reversible exchange (SABRE) parahydrogen-based hyperpolarisation technique to enhance the sensitivity of natural abundance 1D and 2D 13C{1H} benchtop NMR spectra. We compare two detection methods for SABRE-enhanced 13C NMR and observe an optimal 13C{1H} signal-to-noise ratio (SNR) for a refocused INEPT approach, where hyperpolarisation is transferred from 1H to 13C. In addition, we exemplify SABRE-enhanced 2D 13C benchtop NMR through the acquisition of a 2D HETCOR spectrum of 260 mM of 4-methylpyridine at natural isotopic abundance in a total experiment time of 69 min. In theory, signal averaging for over 300 days would be required to achieve a comparable SNR for a thermally polarised benchtop NMR spectrum acquired of a sample of the same concentration at natural abundance.

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“…[36][37][38][39][40][41][42] More importantly, the advent of a number of innovative in-line analytical tools has greatly advanced reaction monitoring and subsequent adjustment of reaction conditions. [43][44][45][46] In this context, an increasing number of new applications have been reported on the use of portable flow IR devices [47][48][49][50] and bench-top low field NMR equipment, [51][52][53][54][55][56] which greatly enabled real-time monitoring of continuous flow chemistry.…”

Section: Introductionmentioning

confidence: 99%

Real-Time Spectroscopic Analysis Enabling Quantitative and Safe Consumption of Fluoroform during Nucleophilic Trifluoromethylation in Flow

Musio

Gala

Ley

2017

ACS Sustainable Chem. Eng.

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The productive use of toxic waste materials derived from industrial processes is one of the main goals of modern chemical research to increase sustainability of the large scale production. Here we devise a simple and robust strategy for the utilization of trifluoromethane, obtained in large quantities from polytetrafluoroethylene (PTFE) manufacture, and the conversion of this greenhouse gas into valuable fluorinated compounds. The generation of the trifluoromethyl carbanion and its direct and complete consumption through trapping with a number of electrophiles were achieved by a fully contained flow reactor setup. The adoption of modern in-line analytical tools, such as portable FT-IR and NMR devices, allowed the accurate reagent dosing with considerable benefits in terms of controlling the environmental impact during this continuous process. The advantages of the method, with respect to the batch procedure, will be discussed and demonstrated experimentally. 2

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Oxidative Neutralization of Mustard‐Gas Simulants in an On‐Board Flow Device with In‐Line NMR Monitoring

Abstract: Scheme 1. Oxidation of mustard gas yperite (HD) into the corresponding sulfoxide (HDO) and sulfone (HDO 2 ).

Cited by 15 publications

References 51 publications

Gradient-based pulse sequences for benchtop NMR spectroscopy

Gradient-based pulse sequences for benchtop NMR spectroscopy

Hyperpolarised 1H–13C Benchtop NMR Spectroscopy

Real-Time Spectroscopic Analysis Enabling Quantitative and Safe Consumption of Fluoroform during Nucleophilic Trifluoromethylation in Flow

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