<i>In situ</i>study of reaction kinetics using compressed sensing NMR

Wu, Yuting; D’Agostino, Carmine; Holland, Daniel J.; Gladden, Lynn F.

doi:10.1039/c4cc06051b

Cited by 38 publications

(31 citation statements)

References 18 publications

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“…There is a need to introduce additional alternative methods to assess newly designed and synthesized molecules when they are not amenable to UVvis interpretations. A recent report using 2D NMR to study reaction kinetics in situ was also highlighted [5]. In this communication, direct 1D 1 H NMR is used to gain reliable relative photorelease information with reproducible results.…”

Section: Introductionmentioning

confidence: 92%

Unambiguous evaluation of the relative photolysis rates of nitro indolinyl protecting groups critical for brain network studies

Comitz

Ouedraogo

Nesnas

2015

Analytical Chemistry Research

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a b s t r a c tNitrated indolinyl photoprotecting groups are crucial tools extensively used in the study of neuronal signal transduction. Mononitrated photolabile protecting groups have been used effectively, however, recent advances in the introduction of a second nitro group have shown improvement in the photo efficiency of neurotransmitter (agonist) release, albeit, to varying extents, depending on the assessment methods employed. An unambiguous method is discussed based on Nuclear Magnetic Resonance (NMR), which is shown to be an effective technique in the relative overall rate comparison amongst varying nitrated protecting groups. Mononitrated and dinitrated photolabile protecting groups such as CDNIGlu and MNI-Glu are used as an example to assess the relative value of adding a second nitro group in photoactive cage designs. Using this technique, it was shown that the second nitro group in CDNI systems enhances the overall relative rate of photocleavage by a factor of 5.8. This reported method can also be used to unambiguously determine relative rate of agonist photorelease.

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Section: Introductionmentioning

confidence: 92%

Unambiguous evaluation of the relative photolysis rates of nitro indolinyl protecting groups critical for brain network studies

Comitz

Ouedraogo

Nesnas

2015

Analytical Chemistry Research

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“…However, a surface modied SW catalyst in a CWPO reaction has not yet been reported, while other carbon materials such as activated carbon, graphene and carbon nanotubes have been widely investigated as surface functional groups. 22 High-resolution mass spectrometry (HRMS), equipped with a weak ionization source such as an electrospray ionization (ESI) source, is useful to identify the accurate molecular formula for mixed organic compounds in a reaction system. It is necessary to study the degradation pathways of cresol in the CWPO reaction in detail since the toxicity of some intermediates can be higher than that of the initial compound.…”

Section: Introductionmentioning

confidence: 99%

Surface modification of sewage sludge derived carbonaceous catalyst for m-cresol catalytic wet peroxide oxidation and degradation mechanism

Yang

Wei

et al. 2015

RSC Adv.

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Sewage sludge derived carbonaceous materials (SWs) treated with different kinds of acid were used as the catalysts for catalytic wet peroxide oxidation (CWPO) of m-cresol in batch reactor and continuous reactor, respectively. The results showed that SW treated with nitric acid (HNO 3 -SW) and sulfuric acid (H 2 SO 4 -SW) exhibited high catalytic activity in a CWPO reaction. The conversion of m-cresol reached 100%, after CWPO reaction for 3 h at an initial pH of 7 and a temperature of 25 C over a H 2 SO 4 -SW catalyst. The elements content and chemical state of SWs treated with different kinds of acids were measured by XRF, XPS and Mössbauer spectra, the results implied that ferric iron and surface functional groups might play the main role in m-cresol degradation. The intermediate oxidation products were identified by in situ NMR, GC-MS, IC and HRMS analyses. Based on a free-radical reaction mechanism, a m-cresol oxidation pathway in CWPO was proposed.

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“…It is possible to reconstruct the TR‐NUS signal with any of the NUS methods used in NMR, applied to each of the subsets separately ,. One method that has become very popular over the past decade is “compressed sensing” (CS) ,,,. CS is based on the assumption, that spectrum is sparse (“almost empty”) and thus can be recovered from small fraction of the data required by Fourier Transform (FT).…”

Section: Figurementioning

confidence: 99%

Monitoring Hydrogenation Reactions using Benchtop 2D NMR with Extraordinary Sensitivity and Spectral Resolution

et al. 2019

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Low‐field benchtop nuclear magnetic resonance (BT‐NMR) spectrometers with Halbach magnets are being increasingly used in science and industry as cost‐efficient tools for the monitoring of chemical reactions, including hydrogenation. However, their use of low‐field magnets limits both resolution and sensitivity. In this paper, we show that it is possible to alleviate these two problems through the combination of parahydrogen‐induced polarization (PHIP) and fast correlation spectroscopy with time‐resolved non‐uniform sampling (TR‐NUS). PHIP can enhance NMR signals so that substrates are easily detectable on BT‐NMR spectrometers. The interleaved acquisition of one‐ and two‐dimensional spectra with TR‐NUS provides unique insight into the consecutive moments of hydrogenation reactions, with a spectral resolution unachievable in a standard approach. We illustrate the potential of the technique with two examples: the hydrogenation of ethylphenyl propiolate and the hydrogenation of a mixture of two substrates – ethylphenyl propiolate and ethyl 2‐butynoate.

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In situstudy of reaction kinetics using compressed sensing NMR

Abstract: CS-NMR improves the temporal resolution of conventional multi-dimensional NMR for species identification and study of reaction kinetics.

Cited by 38 publications

References 18 publications

Unambiguous evaluation of the relative photolysis rates of nitro indolinyl protecting groups critical for brain network studies

Unambiguous evaluation of the relative photolysis rates of nitro indolinyl protecting groups critical for brain network studies

Surface modification of sewage sludge derived carbonaceous catalyst for m-cresol catalytic wet peroxide oxidation and degradation mechanism

Monitoring Hydrogenation Reactions using Benchtop 2D NMR with Extraordinary Sensitivity and Spectral Resolution

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