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Liane K. Soares Renata G. LaraRaquel G. Jacob Eder J. LenardãoDiego Alves Gelson Perin 《Tetrahedron letters》2014
We present herein our results on the nucleophilic addition of imidazole to a range of arylselanylalkynes by simple heating in DMF without any additives to give (Z)-1-(1-organyl-(2-arylselanyl)vinyl)-1H-imidazoles. The reactions were performed under mild conditions with a range of arylselanylalkynes in good yields and with high regio- and stereoselectivity to give the respective (Z)-arylselanyl alkene as the only isomer. 相似文献
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Five new block copoly(imide siloxane)s have been prepared by reacting two different diamines, 4,4″-bis(p-aminophenoxy)-3,3″-trifluoromethyl terphenyl (APTTFT) and amino-propyl terminated polydimethylsiloxane (APPS), separately with 4,4′-(4,4′-isopropylidenediphenoxy)bis(phthalic anhydride); BPADA. The reactions were conducted by a two pot solution imidization technique. The diamine APTTFT and the dianhydride BPADA composed the hard block segment while APPS and BPADA composed the soft block segment. The soft and hard blocks of different block lengths were generated by different stoichiometric imbalance in two different flasks and the final polymers were obtained by reacting both the blocks together. Different block copoly(imide siloxane)s were prepared on increasing the hard block lengths (DP) from 7 to 12, 18, 23 and 28 and the soft block lengths (DP) from 4 to 6, 8, 10 and 12, respectively. The resulting polymers have been well characterized by NMR, DSC and DMA techniques. The properties of the block copolymers were compared with the analogous random copolymers and homopolyimide prepared without APPS. 相似文献
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Several new random and block copoly(imide siloxane)s have been prepared by the solution polycondensation of commercially available 4,4′-oxydianiline (ODA) and amino-propyl terminated polydimethylsiloxane (APPS) with 4,4′-(hexafluoro-isopropylidene)diphthalic anhydride (6FDA). The siloxane loading was kept to 10, 20, 30, 40 and 50 wt% in the copolymers. The random copolymers were prepared by a one pot solution imidization technique, and two pot solution imidization technique was adopted for the synthesis of the block copolymers. The diamine ODA and the dianhydride 6FDA composed the hard block segment, while APPS and 6FDA composed the soft block segment. The hard block length was kept constant while the soft block lengths were varied by varying the siloxane loading. Accordingly, block copoly(imide siloxane)s were prepared on increasing the soft block lengths (DP) from 3 to 6, 10, 18 and 36 for fixed hard block length of 22. The resulting polymers have been well characterized by IR, NMR and GPC techniques. Thermal and mechanical properties of the random and block copolymers were compared with the already reported homopolyimide without siloxane moiety. 相似文献
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R. Benassi C. Bertarini L. Hilfert G. Kempter E. Kleinpeter J. Spindler F. Taddei S. Thomas 《Journal of Molecular Structure》2000,520(1-3):273-294
The structure of a number of 2-exo-methylene substituted quinazolines and benzodiazepines, respectively, 1, 3a,b, 4 (X=–CN,–COOEt) and their 2-cyanoimino substituted analogues 2, 3c,d (X=–CN,–SO2C6H4–Me(p) was completely assigned by the whole arsenal of 1D and 2D NMR spectroscopic methods. The E/Z isomerism at the exo-cyclic double bond was determined by both NMR spectroscopy and confirmed by ab initio quantum chemical calculations; the Z isomer is the preferred one, its amount proved dependent on steric hindrance. Due to the push–pull effect in this part of the molecules the restricted rotation about the partial C2,C11 and C2,N11 double bonds, could also be studied and the barrier to rotation measured by dynamic NMR spectroscopy. The free energies of activation of this dynamic process proved very similar along the compounds studied but being dependent on the polarity of the solvent. Quantum chemical calculations at the ab initio level were employed to prove the stereochemistry at the exo-cyclic partial double bonds of 1–4, to calculate the barriers to rotation but also to discuss in detail both the ground and the transition state of the latter dynamic process in order to better understand electronic, inter- and intramolecular effects on the barrier to rotation which could be determined experimentally. In the cyanoimino substituted compounds 2, 3c,d, the MO ab initio calculations evidence the isomer interconversion to be better described by the internal rotation process than by the lateral shift mechanism. 相似文献
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The compound 2,10-dibromo-3-chloro-8-hydroxy-β-chamigrene was analysed in detail by NMR Spectroscopy. the complete assignment of the signals in the 1H and 13C NMR spectra and the determination of the relative configurations were achieved by 2D NMR techniques, AM1 data and 1H spectrum simulation. Comparisons of the results with related spiro chamigrene systems are also presented. 相似文献
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Christel Hempen Liane Glsle-Schwarz Ulrich Kunz Uwe Karst 《Analytica chimica acta》2006,560(1-2):35-40
Telmisartan is an angiotensin II receptor antagonist and a known drug against high blood pressure. In this report, the development of a new and rapid analytical technique, an enzyme-linked immunosorbent assay (ELISA) for the determination of telmisartan in human blood plasma is described. The immunoassay is based on a conversion of 4-(N-methylhydrazino)-7-nitro-2,1,3-benzooxadiazole (MNBDH) to 4-(N-methylamino)-7-nitro-2,1,3-benzooxadiazole (MNBDA), which is detected by fluorescence spectroscopy. The limit of detection was 0.1 ng/mL, the limit of quantification was 0.3 ng/mL and the working range extended from 0.3 ng/mL to 300 ng/mL. 相似文献
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The partial hydrogenation of benzene to cyclohexene by nanoscale ruthenium catalysts in imidazolium ionic liquids 总被引:3,自引:0,他引:3
Silveira ET Umpierre AP Rossi LM Machado G Morais J Soares GV Baumvol IJ Teixeira SR Fichtner PF Dupont J 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(15):3734-3740
The controlled decomposition of an Ru(0) organometallic precursor dispersed in 1-n-butyl-3-methylimidazolium hexafluorophosphate (BMI.PF(6)), tetrafluoroborate (BMI.BF(4)) or trifluoromethane sulfonate (BMI.CF(3)SO(3)) ionic liquids with H(2) represents a simple and efficient method for the generation of Ru(0) nanoparticles. TEM analysis of these nanoparticles shows the formation of superstructures with diameters of approximately 57 nm that contain dispersed Ru(0) nanoparticles with diameters of 2.6+/-0.4 nm. These nanoparticles dispersed in the ionic liquids are efficient multiphase catalysts for the hydrogenation of alkenes and benzene under mild reaction conditions (4 atm, 75 degrees C). The ternary diagram (benzene/cyclohexene/BMI.PF(6)) indicated a maximum of 1 % cyclohexene concentration in BMI.PF(6), which is attained with 4 % benzene in the ionic phase. This solubility difference in the ionic liquid can be used for the extraction of cyclohexene during benzene hydrogenation by Ru catalysts suspended in BMI.PF(6). Selectivities of up to 39 % in cyclohexene can be attained at very low benzene conversion. Although the maximum yield of 2 % in cyclohexene is too low for technical applications, it represents a rare example of partial hydrogenation of benzene by soluble transition-metal nanoparticles. 相似文献
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Yanan Gao Dr. Andreas Voigt Dr. Liane Hilfert Dr. Kai Sundmacher Prof. 《Chemphyschem》2008,9(11):1603-1609
A common ionic liquid (IL), 1‐butyl‐3‐methylimidazolium tetrafluoroborate (bmimBF4), is used as polar solvent to induce the formation of a reverse bmimBF4‐in‐toluene IL microemulsion with the aid of the nonionic surfactant Triton X‐100. The swelling process of the microemulsion droplets by increasing bmimBF4 content is detected by dynamic light scattering (DLS), conductivity, UV/Vis spectroscopy, and freeze‐fracture transmission electron microscopy (FF–TEM). The results show that the microemulsion droplets initially formed are enlarged by the addition of bmimBF4. However, successive addition of bmimBF4 lead to the appearance of large‐sized microemulsion droplet clusters (200–400 nm). NMR spectroscopic analysis reveal that the special structures and properties of bmimBF4 and Triton X‐100 together with the polar nature of toluene contribute to the formation of such self‐assemblies. These unique self‐assembled structures of IL‐based microemulsion droplet clusters may have some unusual and unique properties with a number of interesting possibilities for potential applications. 相似文献
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Determination of drugs of abuse in blood is of great importance in clinical and forensic toxicology. This review describes
procedures for detection of the following drugs of abuse and their metabolites in whole blood, plasma or serum: Δ9-tetrahydrocannabinol,
11-hydroxy-Δ9-tetrahydrocannabinol, 11-nor-9-carboxy-Δ9-tetrahydrocannabinol, 11-nor-9-carboxy-Δ9-tetrahydrocannabinol glucuronide,
heroin, 6-monoacetylmorphine, morphine, morphine-6-glucuronide, morphine-3-glucuronide, codeine, amphetamine, methamphetamine,
3,4-methylenedioxymethamphetamine, N-ethyl-3,4-methylenedioxyamphetamine, 3,4-methylenedioxyamphetamine, cocaine, benzoylecgonine, ecgonine methyl ester, cocaethylene,
other cocaine metabolites or pyrolysis products (norcocaine, norcocaethylene, norbenzoylecgonine, m-hydroxycocaine, p-hydroxycocaine, m-hydroxybenzoylecgonine, p-hydroxybenzoylecgonine, ethyl ecgonine, ecgonine, anhydroecgonine methyl ester, anhydroecgonine ethyl ester, anhydroecgonine,
noranhydroecgonine, N-hydroxynorcocaine, cocaine N-oxide, anhydroecgonine methyl ester N-oxide). Metabolites and degradation products which are recommended to be monitored for assessment in clinical or forensic
toxicology are mentioned. Papers written in English between 2002 and the beginning of 2007 are reviewed. Analytical methods
are assessed for their suitability in forensic toxicology, where special requirements have to be met. For many of the analytes
sensitive immunological methods for screening are available. Screening and confirmation is mostly done by gas chromatography
(GC)–mass spectrometry (MS) or liquid chromatography (LC)–MS(/MS) procedures. Basic information about the biosample assayed,
internal standard, workup, GC or LC column and mobile phase, detection mode, and validation data for each procedure is summarized
in two tables to facilitate the selection of a method suitable for a specific analytic problem. 相似文献