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Avelina Arnanz Consuelo Moreno Allan J. Lough Salomé Delgado 《Journal of organometallic chemistry》2004,689(20):3218-3231
The reaction between 2,5-bis(trimethylsilylethynyl)thiophene and Co2(CO)8 or Co2(CO)6(X), (X = dppa, dppm), gave rise to the formation of substituted ethynylcobalt complexes containing one or two Co2(CO)6 or Co2(CO)4(X) units, 2-[Co2(CO)4(X){μ2-η2-(SiMe3)C2}]-5-(Me3SiCC)C4H2S (X = 2CO (1), dppa (3) or dppm (4)) and 2,5-[Co2(CO)4(X){μ2-η2-SiMe3C2}]2C4H2S (X = 2CO (2), dppa (5) or dppm (6)). Desilylation of the non-metallated and metallated alkynes in 3, 4 and 6 occurred on treatment with KOH and tetrabutylammonium fluoride to give 2-[Co2(CO)4(μ-X){μ2-η2-SiMe3C2}]-5-(CCH)C4H2S (X = dppa (7), dppm (8)) and 2,5-[Co2(CO)4(μ-dppm){μ2-η2-HC2}]2C4H2S (9), respectively. Crystals of 6 suitable for single-crystal X-ray diffraction were grown and the molecular structure of this compound is discussed. A comparative electrochemical study of all these complexes is presented by means of the cyclic and square-wave voltammetry techniques. 相似文献
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Avelina Ong-Lee Leo Sylvester Jan W. F. Wasley 《Journal of heterocyclic chemistry》1983,20(6):1565-1569
1,3,4,14b-Tetrahydro-2H,10H-pyrazino[1,2-α]pyrrolo[2,1-c] [1,4]benzodiazepines (1a-e) were synthesized to investigate their potential CNS activity. The key step in the synthesis was the formation of the 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine (13) by reduction and concomitant cyclization of the nitroketone (11). Biological evaluation of 1a-e revealed interesting properties for 1b (CGS 7525A) [2]. 相似文献
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Susan C. Scott Nicole M. Anders Ping He Avelina Hemingway Steven D. Gore Christine L. Hann Michelle A. Rudek 《Biomedical chromatography : BMC》2022,36(3):e5289
The Bcl-2 family small molecule inhibitor navitoclax is being clinically evaluated to treat multiple cancers including lymphoid malignancies and small cell lung cancer. A sensitive and reliable method was developed to quantitate navitoclax in human plasma using liquid chromatography with tandem mass spectrometry with which to perform detailed pharmacokinetic studies. Sample preparation involved protein precipitation using acetonitrile. Separation of navitoclax and the internal standard, navitoclax-d8, was achieved with a Waters Acquity UPLC BEH C18 column using isocratic flow over a 3 min total analytical run time. A SCIEX 4500 triple quadrupole mass spectrometer operated in positive electrospray ionization mode was used for the detection of navitoclax. The assay range was 5–5,000 ng/ml and proved to be accurate (89.5–104.9%) and precise (CV ≤ 11%). Long-term frozen plasma stability for navitoclax at −70°C was at least 43 months. The method was applied for the measurement of total plasma concentration of navitoclax in a patient receiving a 250 mg daily oral dose. 相似文献
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Intramolecular Cyclization of Butadiyne Functionalized Ligands coordinated to Triosmium‐Carbonyl Cluster 下载免费PDF全文
Avelina Arnanz Rosa‐María Medina María‐José Macazaga Consuelo Moreno 《无机化学与普通化学杂志》2016,642(19):1104-1111
Reactions between diynes and [Os3(CO)11(CH3CN)] in the presence of water give rise to the formation of intriguing hydride triosmium clusters [Os3(μ‐H)(CO)9{μ3,η1:η3:η1‐RC2COHC≡CR}] ( 1a – 1c ) under mild conditions in high yields. When these allylic alcohol compounds 1a – 1c are dissolved in dry polar and donor solvents, an intramolecular cyclization process takes place to give [Os3(μ‐H)(CO)9{μ3,η1:η3:η1‐RC2CH=COCR}] ( 2a – 2c ) in quantitative yield. The utilization of [Os3(CO)11(CH3CN)] as starting material together with the addition of water can replace the inconvenient use of [Os3(μ‐H)2(CO)10]. This method of synthesis provides a facile pathway for diyne cyclizations and has a clear advantage over those described to date in the literature. Additionally, the analogous cyclized mixed‐metal complex [Os3(μ‐H)(CO)9{μ3,η1:η3:η1‐FcC2CH=COCFc}] ( 2d ) (Fc = ferrocenyl), was synthesized in order to carry out a comparative electrochemical study with the related compounds [Os3(CO)11(μ3‐FcC4Fc)] ( I ) and [Os3(CO)10(μ3‐FcC4Fc)] ( II ), which were previously reported by R. D. Adams. 相似文献
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Villaverde G Arnanz A Iglesias M Monge A Sánchez F Snejko N 《Dalton transactions (Cambridge, England : 2003)》2011,40(37):9589-9600
Chiral compounds prepared from proton sponge building block 8-((2R,5R)-2,5-dimethylpyrrolidin-1-yl)naphthalen-1-amine were found to be effective chiral ligands for obtaining complexes of rhodium(I) and palladium(II) by reaction with [RhCl(cod)](2), PdCl(2)(cod) or Pd(OAc)(2). The complexes bearing triethoxysilane groups were immobilized on mesoporous MCM-41 in order to obtain new heterogeneous catalysts. Both materials are active in the hydrogenation of alkenes and could be recycled without loss of activity or enantioselectivity. 相似文献
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Avelina Arnanz Salomé Delgado Consuelo Moreno 《Journal of organometallic chemistry》2008,693(23):3457-3470
A large number of Co2(CO)6- and Co2(CO)4(L-L)-substituted alkyne complexes (L-L = dppa and dmpm) have been prepared, characterized and studied by cyclic and square-wave voltammetry. In this paper we report a comparative electrochemical study of 2,5-, 2,4-, 3,4- and 2,3-bis(trimethylsilylethynyl)thiophene dicobalt substituted alkyne complexes, in order to evaluate the extent of the electronic interaction between the “Co2C2” redox centres depending on the position of the alkynyl substituent on the thiophene ring. 相似文献
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Mosqueda Y Pomares M Pérez-Cappe EL Miranda A Fariñas JC Larrea MT 《Analytical and bioanalytical chemistry》2006,386(6):1855-1862
An analytical method was developed for the determination of three major (Li, Ni and Co) and fourteen minor or trace elements
(Al, Ba, Ca, Cu, Cr, Fe, K, Mg, Mn, Na, Si, Sr, Ti and V) in LiNi1−x
Co
x
O2 (x = 0.2–0.8) ceramic powders by inductively coupled plasma optical emission spectrometry. Sample dissolution was achieved by
25% nitric acid digestion in a microwave oven. For each element, an analytical line free from spectral interferences was selected.
A detailed study of matrix effects over a wide interval of total excitation energy (TEE) lines (1.62–16.50 eV) was performed
at near-robust plasma conditions. A remarkable enhancement in atomic lines with TEE <4 eV was noticed, whereas a significant
reduction in atomic and ionic lines with TEE >4 eV was observed. The extrapolation to infinite dilution method was successfully
used to overcome these nonspectroscopic interferences. Detection limits (3σ) varied from 0.21 mg kg−1 for Sr to 49.7 mg kg−1 for Na. The precision of determination (obtained as the relative standard deviation) was lower than 1% for the major elements
Li, Ni and Co and between 0.69 and 10% for minor and trace elements. The accuracy of the method ranged from 91 to 101% for
major elements, and from 90 to 110%, or close to this range, for most of the impurities in both of the samples studied.
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