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1.
Summary A detector for microchromatography in which Raman spectroscopy is used to identify the eluted species has been developed.
The detector is designed to be applicable to a wide range of compounds without requiring the presence of a chromophore. Its
use is illustrated in the analysis of nitro compounds on a 250 μm i.d. column. Raman spectra of each of the compounds could
be identified as they passed the detector. The advatages of the use of fully deuterated solvents are demonstrated by the analysis
of nitrobenzenes in methanol/water mobile phases. The detection limit for nitrobenzene using the Raman line at 1342 cm−1 was 75ng. 相似文献
2.
The microwave-assisted synthesis of 5-amino-3-aralkoxy(methoxy)amino-1,2,4-oxadiazoles starting from N1-aralkoxy-(methoxy)-N3-cyano-O-phenylisoureas and hydroxylamine is described. N1-Aralkoxy(methoxy)-N3-cyano-O-phenylisoureas are readily accessible by treatment of diphenyl N-cyanimidocarbonate with O-substituted hydroxylamines. 相似文献
3.
Nariman M. A. Nahas 《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):2327-2335
Thermal fragmentation of O-Aryl-N,N-diphenylhydroxylamines I and II were investigated. Neat heating in an atmospheric nitrogen afforded arenes, biaryl, diaryl sulfide, diphenylamine, diaryl sulfone, phenols, arenesulfonic acid, carbazole, and thianthrene. In the presence of isoquinoline as a radical trap, I gave 1-phenylisoquinoline as well as the previous products. Analogous results were obtained on heating of I in boiling tetraline, which lead to the formation of 1-hydroxytetraline, α -tetralone, and 1,1′-bitetralyl as the major products. A free-radical mechanism has been postulated to take place through the initial homolysis of N─O and S─O bonds to account for the identified products. 相似文献
4.
Ptaquiloside, a potent carcinogen present in bracken fern, a plant consumed by farm animals, may be detected in traces by converting it into the bromopterosine. A simple synthesis of bromopterosine d2, to be used as standard in GC/MS or LC/MS analyses, is described. 相似文献
5.
Abil E. Aliev Alex J. Sinclair Shen Zhou John D. Wilden Stephen Caddick Dimitri M. Kullmann Dmitri A. Rusakov 《Journal of Physical Organic Chemistry》2009,22(6):607-612
While developing a synthesis towards tagged dizocilpine (MK‐801) analogues, we observed highly restricted inversion of a nitrogen centre in a number hydroxylamines obtained as key intermediates. These compounds are shown to possess some of the structural elements which are expected to significantly hinder the nitrogen inversion, potentially leading to hydroxylamines with a chiral nitrogen centre. Free energy barriers (ΔG≠) of the nitrogen inversion were estimated to be ca. 22 kcal mol?1 at temperatures near 420 K using variable temperature NMR measurements in DMSO‐d6. Further density functional studies of a number model systems were undertaken in order to better rationalize the measured inversion barriers and follow the role of various structural factors in raising the barrier height of the nitrogen inversion process. Copyright © 2008 John Wiley & Sons, Ltd. 相似文献
6.
A. V. Varlamov D. G. Grudinin A. I. Chernyshev A. N. Levov N. I. Golovtsov R. S. Borisov 《Chemistry of Heterocyclic Compounds》2001,37(3):346-352
4,5-Dihydro-5-methyl-3H-spiro[benz-2-azepine-3-cyclohexane] N-oxide reacted with cyanide ion and isopropyl magnesium bromide to give the corresponding 1-cyano- and 1-isopropyl-4,5-dihydro-5-methyl-3H-spiro[benz-2-azepine-3-cyclohexane], but reaction with phenyl magnesium bromide, benzyl magnesium chloride, and nitromethane gave cyclic hydroxylamines: 1-substituted N-hydroxy-1,2,4,5-tetrahydro-5-methyl-3H-spiro[benz-2-azepine-3-cyclohexanes] which were oxidized to the corresponding nitrones. 相似文献
7.
Tertiary aliphatic β- and γ-nitro nitriles and ketones deuterated in (several) selected positions had been synthesized. The deuterated nitro compounds served as a starting material for the corresponding deuterium labeled nitrones or hydroxylamines (reducing with aluminum amalgam). Further oxidation of the last two groups of compounds with sodium periodate or m-CPBA afforded the relevant deuterated tertiary C-nitroso compounds. 相似文献
8.
The Fourier transform infrared (FTIR) absorption spectrum of the ν12 fundamental band of ethylene-d4 (C2D4) was recorded in the 1017-1137 cm−1 region with an unapodized resolution of 0.0063 cm−1. Upper state (v12 = 1) rovibrational constants consisting of three rotational and five quartic constants were improved by assigning and fitting 2103 infrared transitions using Watson’s A-reduced Hamiltonian in the Ir representation. The band centre of the A-type ν12 band is found to be 1076.98480 ± 0.00002 cm−1. The present analysis covering a wider wavenumber range and higher J and Kc values yielded upper state constants including the band centre which are more accurate than previously reported. The rms deviation of the upper state fit is 0.00045 cm−1. Improved ground state rovibrational constants were also determined from the fit of 1247 ground state combination differences (GSCD) from the presently-assigned infrared transitions of the ν12 band of C2D4. The rms deviation of the GSCD fit is 0.00049 cm−1. In the rovibrational analysis, local frequency perturbations were not detected even at high J and Ka values. The calculated inertial defect Δ12 is 0.32551 ± 0.00001 μÅ2. The line intensities of the individual transitions in the ν12 band were measured and the band strength of 39.8 ± 2.0 cm−2 atm−1 was derived for the ν12 band of C2D4. 相似文献
9.
The absorption spectrum of dideuterated water, D2O, has been recorded between 8800 and 9520 cm−1 by intracavity laser absorption spectroscopy (ICLAS) based on a vertical external cavity system emitting laser (VeCSEL) and by high sensitivity Fourier Transform spectroscopy. The combined analysis of the spectra has allowed attributing 1223 transitions to the D2O species. The spectrum assignment was performed on the basis of the recent results of variational calculations based on an optimized potential energy surface of D2O. A set of 687 energy levels was derived from transitions assigned to eight upper vibrational states, 577 of them being reported for the first time. A detailed line list has been generated. The line intensities were retrieved mainly from the FTS spectrum and the absolute integrated intensities of the 2v1 + v2 + v3 and the v2 + 3v3 bands dominating the spectrum have been determined. 相似文献
10.
Ning Yu Jing-Fang Lv Shi-Mei He Yanyan Cui Ye Wei Kun Jiang 《Molecules (Basel, Switzerland)》2022,27(23)
In the presence of CuOAc, a series of unsymmetric ureas can be generated in moderate to good yields under mild reaction conditions (10 mol% of CuOAc, 2 equiv t-BuONa or PhONa, 30 °C), using aryl isocyanides and O-benzoyl hydroxylamines as the readily accessible starting materials. The reactions might undergo a cascade process involving isocyanide insertion into the N-O bond and Mumm-type rearrangement. This work represents a rare example of isocyanide insertion into N-O bonds, which would extend isocyanide insertion chemistry. 相似文献