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A series of chiral oxovanadium(IV) complexes derived from tridentate N-3,5-substituted and N-3,4-benzo- and N-5,6-benzo-salicylidene-alpha-amino acids can serve as efficient catalysts for the enantioselective oxidative couplings of various 3-, 6-, and 7-substituted 2-naphthols under O(2). The best scenario involves the use of a vanadyl complex arising from 2-hydroxy-1-naphthaldehyde and valine (or phenylalanine) in CCl(4), leading to BINOLs in good yields (75-100%) and with enantioselectivities of up to 68%. 相似文献
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Satheeshmanikandan RS Thappali Kanthikiran VS Varanasi Sridhar Veeraraghavan Swaroop Kumar VS Vakkalanka Mukkanti K 《Journal of mass spectrometry : JMS》2012,47(12):1612-1619
A sensitive and reliable high‐performance liquid chromatography–mass spectrometry (LC–MS/MS) was developed and validated for simultaneous quantification IC87114, roflumilast (RFM), and its active metabolite roflumilast N‐oxide (RFN) using tolbutamide as an internal standard. The analytes were extracted by using liquid–liquid extraction and separated on a reverse phase C18 column (50 mm × 3 mm i.d., 4.6 µ) using methanol: 2 mM ammonium acetate buffer, pH 4.0 as mobile phase at a flow rate 1 mL/min in gradient mode. Selective reaction monitoring was performed using the transitions m/z 398.3 > 145.9, 403.1 >186.9, 419.1 > 187.0 and 271.1 > 155.0 to quantify quantification IC87114, RFM, RFN and tolbutamide, respectively. The method was validated over the concentration range of 0.1–60 ng.mL?1 for RFM and RFN and 6 to 2980 ng.mL?1 for IC87114. Intra‐ and inter‐day accuracy and precision of validated method were within the acceptable limits of <15% at all concentrations. Coefficients of correlation (r2) for the calibration curves were >0.99 for all analytes. The quantitation method was successfully applied for simultaneous estimation of IC87114, RFM and RFN in a pharmacokinetic drug–drug interaction study in Wistar rats. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Munshi G Mustafa Sudhir Raniwala T Awes B Rai RS Bhalerao JG Contreras RV Gavai SK Ghosh P Jaikumar GC Mishra AP Mishra H Mishra B Mohanty J Nayak J-Y Ollitrault SC Phatak L Ramello R Ray PK Sahu AM Srivastava DK Srivastava VK Tiwari 《Pramana》2006,67(5):961-981
This is the report of Heavy Ion Physics and Quark-Gluon Plasma at WHEPP-09 which was part of Working Group-4. Discussion and
work on some aspects of quark-gluon plasma believed to have created in heavy-ion collisions and in early Universe are reported. 相似文献
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A.V Barhate V.B Sapre Chintamani Mande 《Journal of Physics and Chemistry of Solids》1982,43(8):761-765
Chemical shifts of the X-ray LIII absorption discontinuities of rhenium in some of its binary and ternary compounds have been studied using a bent crystal X-ray spectrograph. The chemical shifts (ΔE) are found to be governed by the effective charges (q) on the absorbing ions, which have been calculated using Suchet's theory. For the compound ReCl5, however, the effective ionic charge cannot be calculated since the pentavalent radius of rhenium is not known. The ΔE, q plot has been used to determine the charges on the rhenium ions in ReCl5 as well as in two ternary compounds KReO4 and NaReO4. Our work has enabled us to determine the ionic radius of pentavalent rhenium. 相似文献
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The authors have reanalysed the data on the EXAFS associated with the rhenium LIII absorption discontinuity in the metal and in some of its compounds, and have interpreted them in the light of the recent theory proposed by Lytle, Sayers and Stern. It has been shown that the α parameter of EXAFS is a measure of valency and that the metallic valency of rhenium is two. 相似文献
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Chandan L. Barhate M. Farooq Wahab Zachary S. Breitbach David S. Bell Daniel W. Armstrong 《Analytica chimica acta》2015
State of the art chiral chromatography still employs 3–5 μm bonded or immobilized chiral selectors in 10–25 cm columns. With the availability of 1.9 μm narrow particle size distribution (NPSD) silica, it is now possible to make ever shorter, high efficiency columns practical for sub-minute chiral separations. Three macrocyclic glycopeptides (teicoplanin, teicoplanin aglycone, and vancomycin) were bonded onto 1.9 μm NPSD particles. Such packed columns had ∼80% lower backpressure as compared to polydisperse (PD) 1.7 μm silica materials when using the same mobile phase. The decreased backpressure allowed for diminution of frictional heating and allowed for the use of the 1.9 μm NPSD particle based columns at high flow rates. The 1.9 μm NPSD particle based columns showed up to 190,000 plates m−1 for chiral molecules and 210,000 plates m−1 for achiral probes. Representative enantiomeric separations are shown for wide classes of compounds, including different types of amino acids, β-blockers, and pharmaceutically important heterocyclic compounds such as oxazolidinones. Applications in three liquid chromatography modes, namely, reversed phase, polar organic mode and normal phase chiral separations were shown with resolution values ranging from 1.5 to 5.7. Additionally, the same columns were used with supercritical fluid chromatography (SFC) for ultrafast separations. 相似文献
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[reaction: see text] A series of oxovanadium(IV) complexes derived from tridentate N-ketopinidene-alpha-amino acids were synthesized. They serve as efficient catalysts for the enantioselective oxidative couplings of various 3-, 6-, or 7-substituted 2-naphthols. The best scenario involves the use of a vanadyl complex arising from L-tert-leucine in CCl4. The asymmetric couplings of 2-naphthols can be conducted smoothly at 40-45 degrees C under a stream of gaseous oxygen, leading to 2,2'-dihydroxy-1,1'-binaphthyls in good yields (61-99%) and with enantioselectivities of up to 87%. 相似文献
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