Search results for "benzen"
showing 10 items of 1735 documents
Isolation of Free Phenylide-like Carbanions with N-Heterocyclic Carbene Frameworks
2009
A series of 1,3-bis(2,6-diisopropylphenyl)-5-methyl-1,3-diaza-4,6-diborabenzenes with methyl, phenyl, and dimethylamino substituents on the ring boron atoms were prepared using the cyclocondensation reaction between N,N'-bis(2,6-diisopropylphenyl)trimethylsilylformamidine and the appropriately substituted 1,1-bis(organochloroboryl)ethane, followed by deprotonation of the cationic ring intermediate. The planar, heterocyclic benzene analogues could be further deprotonated at the other ring carbon using an additional equivalent of potassium hexamethyldisilazide to yield organometallic derivatives akin to the potassium phenylide. The potassium cations could be efficiently sequestered in both so…
Organotin(IV) complexes ofN-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycine
2003
Organotin(IV) derivatives of N-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycine have been synthesized and characterized by 1H, 13C, 119Sn NMR, 119Sn Mossbauer, and IR spectroscopy along with elemental analyses. The di- and triorganotin(IV) complexes were readily obtained from the reactions of organotin halides and sodium/potassium N-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycinate. The diorganotin compound reacted with Ph3SnCl in refluxing benzene to give the mixed organotin dinuclear complex of composition Ph2Sn(2-OC(CH3)-C(H)C(CH3)NCH2COO)·Ph3SnCl, which was characterized by single crystal X-ray structure determination. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 14:149–154, 2003; Publ…
A statistical study of the additivities of substituent effects in the13C NMR chemical shifts of hydroxy- and chloro-substituted benzenes
1980
The 13C NMR spectra of six hydroxybenzenes, all chlorobenzenes, all chlorophenols and eight chlorocatechols are measured and assigned. The additivity of the substituent effects and the usefulness of some corrective parameters are studied with regression analysis. The order of the chemical shifts is most efficiently predicted by the simplest substituent effect model, containing only the direct effects of the substituents, although the 95% confidence limits of the calculated shifts are as high as 5.6 ppm. If the chemical shifts need to be predicted within the measuring errors (approximately 0.05–0.10 ppm, in the present data), the number of necessary corrections is very impractical. The corre…
Reaction of complex ligands: Part 95. Chromium tricarbonyl complexes of polysubstituted naphthohydroquinones: regioselective synthesis via [3+2+1]-be…
2003
Abstract A series of polysubstituted naphthohydroquinoid tricarbonyl chromium complexes were prepared by chromium mediated [3+2+1]-benzannulation of Fischer-type carbene complexes with alkynes. The kinetics and the thermodynamic data of the η6-η6-haptotropic rearrangements were investigated by in-situ NMR spectroscopy. The free activation energies ΔG# range from 23 to 26 kcal mol−1 and only slightly depend on the bulk and the donor/acceptor properties of the substituents. Equilibrium of metal migration was observed for naphthohydroquinone complexes bearing methoxy substituents at the non-hyroquinoid ring (ring A). In complexes bearing methyl groups or only hydrogen substituents at ring A th…
Assessing air quality inside vehicles and at filling stations by monitoring benzene, toluene, ethylbenzene and xylenes with the use of semipermeable …
2007
BTEX (benzene, toluene, ethylbenzene, and xylenes) were used as target molecules to evaluate the quality of air inside motor vehicles and near filling stations, using semipermeable membrane devices (SPMDs) as low-cost passive sampling devices. A direct, fast, simple methodology based on the use of headspace-gas chromatography-mass spectrometry detection (HS-GC-MS) was developed for BTEX determinations, without any sample pre-treatment. SPMDs (25.4 cm2 surface, filled with 100 microL triolein) were employed as static samplers. After the selected deployment time, the SPMDs were heated inside a HS vial at 150 degrees C for 20 min and BTEX compounds were determined by GC-MS in selected ion moni…
Determination of organochlorine pesticide residues in honey from the central zone of Portugal and the Valencian community of Spain
2004
In this study nine organochlorine pesticide residues ([alpha]-, [beta]-, and [gamma]-hexachlorocyclohexane (HCH), hexachlorobenzene (HCB), aldrin, p,p'-DDE, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in forty nine samples of honey collected from markets of Portugal and Spain during 2001 and 2002, respectively, were evaluated. For this evaluation, three analytical procedures were studied. The analytical procedure, based on LLE extraction with ethyl acetate followed by gas chromatography-electron-capture detection (GC-ECD) for quantification, and mass spectrometry (GC-MS) for confirmation, has been selected. Recoveries of spiked samples ranged from 68%, for [beta]-HCH, and 126% for p,p'-DDT, for forti…
Biogenic synthesis of palladium nanoparticles using Pulicaria glutinosa extract and their catalytic activity towards the Suzuki coupling reaction.
2014
Green synthesis of nanomaterials finds the edge over chemical methods due to its environmental compatibility. Herein, we report a facile and eco-friendly method for the synthesis of palladium (Pd) nanoparticles (NPs) using an aqueous solution of Pulicaria glutinosa, a plant widely found in a large region of Saudi Arabia, as a bioreductant. The as-prepared Pd NPs were characterized using ultraviolet-visible (UV-vis) spectroscopy, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), and Fourier transform-infrared spectroscopy (FT-IR). The hydroxyl groups of the plant extract (PE) molecules were found mainly responsible for the red…
Approaches to characterise chromatographic column performance based on global parameters accounting for peak broadening and skewness.
2009
Peak broadening and skewness are fundamental parameters in chromatography, since they affect the resolution capability of a chromatographic column. A common practice to characterise chromatographic columns is to estimate the efficiency and asymmetry factor for the peaks of one or more solutes eluted at selected experimental conditions. This has the drawback that the extra-column contributions to the peak variance and skewness make the peak shape parameters depend on the retention time. We propose and discuss here the use of several approaches that allow the estimation of global parameters (non-dependent on the retention time) to describe the column performance. The global parameters arise f…
Synchronized gradient elution in capillary liquid chromatography
2013
Abstract The synchronization of injection valve operation and gradient elution in capillary liquid chromatography (cHPLC) is studied. Focus is placed on the cHPLC systems which rely on the splitting of a primary flow to provide the much smaller secondary flow required at the injection device and analytical column. Owing to the tiny secondary flow rates, synchronization is necessary to achieve proper optimization of gradient elution methods. Otherwise, there is a risk of having the analytes totally or partially eluted in the initial isocratic conditions, and there is no control on the actual gradient profile reaching the column. Synchronization is first achieved by switching back the valve t…
Glass-capillary gas chromatography of chlorobenzenes on SE-30 and Carbowax 20M columns. Simultaneous determination of chlorobenzenes and chlorophenols
1983
Gas chromatography of benzene and all chlorobenzenes has been studied on SE-30 and Carbowax 20M glasscapillary columns under various operating conditions. The benzene isomers are eluted on both columns according to their boiling points. Separation of all components in a mixture is achieved on Carbowax 20M, whereas on SE-30 the peaks of closely related isomers overlapped. Also one partial overlapping is observed on a non-polar phase. The relative retention times for compounds are given and the retention order is discussed. The retention behaviour of chlorobenzenes and chlorophenols is compared. By using an SE-30 quartz-capillary column a mixture of 33 individual components gives 29 resolved …