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Syntheses of steroidal heterocycles containing a five-membered N,S- heterocycle attached at the 6,7 positions of the B ring are reported. 5Alpha-cholestane-6-one (1), its 3beta-acetoxy- (2) and 3beta-chloro- (3) analogues reacted with semicarbazide and aqueous sodium acetate in refluxing ethanol to yield 5alpha-cholestan-6-one-semicarbazone 1a and its 3-beta-acetoxy and 3beta-chloro derivatives 2a and 3a, respectively. The reactions of 1a, 2a and 3a with thionyl chloride in dichloromethane at low temperature afforded the cyclized thiadiazole 4 and its 3beta-acetoxy- and 3beta-chloro analogues 5 and 6 in good yields. 相似文献
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Stabilization of Catalytically Active Cu+ Surface Sites on Titanium–Copper Mixed‐Oxide Films 下载免费PDF全文
Dr. Ashleigh E. Baber Dr. Xiaofang Yang Dr. Hyun You Kim Dr. Kumudu Mudiyanselage Markus Soldemo Dr. Jonas Weissenrieder Dr. Sanjaya D. Senanayake Dr. Abdullah Al‐Mahboob Dr. Jerzy T. Sadowski Dr. Jaime Evans Dr. José A. Rodriguez Dr. Ping Liu Dr. Friedrich M. Hoffmann Dr. Jingguang G. Chen Dr. Darío J. Stacchiola 《Angewandte Chemie (International ed. in English)》2014,53(21):5336-5340
The oxidation of CO is the archetypal heterogeneous catalytic reaction and plays a central role in the advancement of fundamental studies, the control of automobile emissions, and industrial oxidation reactions. Copper‐based catalysts were the first catalysts that were reported to enable the oxidation of CO at room temperature, but a lack of stability at the elevated reaction temperatures that are used in automobile catalytic converters, in particular the loss of the most reactive Cu+ cations, leads to their deactivation. Using a combined experimental and theoretical approach, it is shown how the incorporation of titanium cations in a Cu2O film leads to the formation of a stable mixed‐metal oxide with a Cu+ terminated surface that is highly active for CO oxidation. 相似文献
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Nanorod vanadatesulfuric acid (VSA NRs), as a recyclable and eco-benign catalyst, was used for one-pot synthesis of 2,4,5-trisubstituted imidazoles and 1,2,4,5-tetrasubstituted imidazoles using aldehydes, benzil, benzoin or 9,10-phenanthrenequinone and ammonium acetate or aniline under solvent-free conditions providing high to excellent yields. VSA is easily prepared by a simple reaction of chlorosulfonic acid and sodium metavanadate in high purity. As compared with the conventional procedures, the present protocol offers several advantages such as simplicity of procedure, short reaction time, high yields, easy workup, recoverability and reusability of the catalyst and simple purification of the products. 相似文献
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Muhammad Imran Malik Tooba Mahboob Shakil Ahmed 《Analytical and bioanalytical chemistry》2014,406(25):6311-6317
Poly(2-vinylpyridine)s (P2VPs) are important polymers with extensive applications in modern day material science. P2VP is an exceptional case for liquid chromatography because of certain polar interactions with most of the stationary phases. In the present study, we established the critical adsorption point (CAP) of P2VP for the first time. The effectiveness of the method is demonstrated by analyses of blends and block copolymers of P2VP and PMMA. The CAP of PMMA is established for determination of molar mass of P2VP component of above mentioned blends and block copolymers. The methods successfully demonstrate the separation of both types of homopolymers from the rest of the samples in conjunction with the determination of molar mass distribution of noncritical block or component. Graphical Abstract
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Asghar Mardani Mohammad Reza Afshar Mogaddam Mir Ali Farajzadeh Ali Mohebbi Mahboob Nemati Mohammadali Torbati 《Journal of separation science》2020,43(18):3674-3682
A sample pretreatment method based on the combination of a three‐phase solvent extraction system and deep eutectic solvent‐based dispersive liquid–liquid microextraction has been introduced for the extraction of four organochlorine pesticides in cocoa samples before their determination by gas chromatography‐electron capture detection. A mixture of sodium chloride, acetonitrile, and potassium hydroxide solution is added to cocoa bean or powder. After vortexing and centrifugation of the mixture, the collected upper phase (acetonitrile) is removed and mixed with a few microliters of N,N‐diethanol ammonium chloride: pivalic acid deep eutectic solvent. Then it is rapidly injected into deionized water and a cloudy solution is obtained. Under optimum conditions, the limits of detection and quantification were found to be 0.011‐0.031 and 0.036‐0.104 ng/g, respectively. The obtained extraction recoveries varied between 74 and 92%. Also, intra‐ (n = 6) and interday (n = 4) precisions were less than or equal to 7.1% for the studied pesticides at a concentration of 0.3 ng/g of each analyte. The suggested method was applied to determine the studied organochlorine pesticide residues in various cocoa powders and beans gathered from groceries in Tabriz city (Iran) and aldrin and dichlobenil were found in some of them. 相似文献
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Mahboob Nemati Mir Ali Farajzadeh Ali Mohebbi Fariba Khodadadeian Mohammad Reza Afshar Mogaddam 《Journal of separation science》2020,43(6):1119-1127
A stir bar sorptive extraction method coupled with deep eutectic solvent based solidification of floating organic droplets–dispersive liquid–liquid microextraction has been used for the simultaneous derivatization and extraction of some acidic pesticides in tomato samples. In this method, initially the analytes are adsorbed on a coated stir bar from tomato juice filled in a narrow tube. After extraction, the stir bar is removed and a water–miscible deep eutectic solvent is used to elute the analytes. Afterward, a derivatization agent and a water–immiscible deep eutectic solvent (as an extraction solvent) with melting point near to room temperature are added to the obtained eluant at µL–levels and the obtained mixture is rapidly injected into deionized water. Under the optimum conditions, the introduced method indicated high enhancement (1543–3353) and enrichment (2530–2999) factors, low limits of detection (7–14 ng/L) and quantification (23–47 ng/L), good linearity (r2 ≥ 0.9982), and satisfactory repeatabilities (relative standard deviation ≤12% for intra– and inter–day precisions at a concentration of 100 ng/L of each analyte). Finally, the proposed method was applied in analysis of the analytes in tomato samples. 相似文献
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In this paper we give a classification of plane symmetric static space-times using symmetry method. For this purpose we consider the Lagrangian corresponding to the general plane symmetric static metric in the Noether symmetry equation. This provides a system of determining equations. Solutions of this system give us classification of the plane symmetric static space-times according to their Noether symmetries. During this classification we recover all the results listed in Feroze et al. (J. Math. Phys. 42:4947, 2001) and Bashir and Ehsan (Il Nuovo Cimento B 123:1, 2008). 相似文献
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Faezeh Javanbakht Mohammad Reza Afshar Mogaddam Mahboob Nemati Mir Ali Farajzadeh 《Journal of separation science》2023,46(8):2200696
In this work, for the first time, a polymeric composite based on β-cyclodextrin grafted with polyethylene has been prepared through ball milling and used as an efficient sorbent for dispersive solid phase extraction of metronidazole and clarithromycin from plasma samples. The prepared sorbent was characterized using Fourier transform infrared spectrophotometry, X-ray diffraction, and scanning electron microscopy. In the extraction process, after precipitating the proteins, the sorbent was added into the sample solution, and the mixture was vortexed to facilitate and speed up the sorption of the analytes onto the sorbent surface. After centrifuging, the sorbent particles were contacted with methanol to elute the analytes under the vortexing process. After this step, an aliquot of the eluate was taken and injected into high-performance liquid chromatography–diode array detector for quantitative analysis. Under the optimum extraction conditions, the extraction recoveries for metronidazole and clarithromycin were 76 and 83%, respectively. The limits of detection were 2.6 and 2.2 ng/ml for metronidazole and clarithromycin, respectively. The repeatability of the offered approach, expressed as relative standard deviation, was equal to or less than 4.7%. Finally, the method was successfully applied to plasma samples of the patients treated with metronidazole and clarithromycin. 相似文献
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Elnaz Marzi Khosrowshahi Behnaz Limuie Khosrowshahi Mir Ali Farajzadeh Abolghasem Jouyban Mustafa Tuzen Mohammad Reza Afshar Mogaddam Mahboob Nemati 《Biomedical chromatography : BMC》2022,36(7):e5371
A dispersive solid-phase extraction method based on a new sorbent has been performed on plasma and wastewater samples to determine metoprolol by high-performance liquid chromatography–tandem mass spectrometry. In this study, the analyte was adsorbed from the samples onto microcrystalline cellulose as a green and efficient sorbent and then eluted for use in the determination step. In the mass spectrometer, the analyte was detected in the positive mode and selectivity of the analysis was increased by sequential mass analysis through multiple reaction monitoring. All of the effective parameters in the extraction of metoprolol from plasma and wastewater were optimized. Under optimal conditions the method was linear in the ranges of 1–1,000 and 0.1–1,000 ng/ml in plasma and wastewater samples, respectively. The detection limits of the method were 0.30 and 0.03 ng/ml in plasma and wastewater samples, respectively. The data showed that the method provides low detection limit, wide linear range, good precision and high extraction recovery. Finally several plasma and wastewater samples were successfully analyzed using the method. The use of a small amount of a green and inexpensive sorbent and a low volume of plasma without the need for further pretreatment steps are the main advantages of the method. 相似文献