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991.
The cyclization of 1‐amino‐2‐mercapto‐5‐[1‐(4‐ethoxyphenyl)‐5‐methyl‐1,2,3‐triazol‐4‐yl]‐1,3,4‐triazole which was synthesized from p‐ethoxyaniline with various triazole acid in absolute phosphorus oxychloride yields 3,6‐bis(1,2,3‐triazolyl)‐s‐triazolo[3,4‐b]‐1,3,4‐thiadiazole derivatives 9a?j , and their structures are established by MS, IR, CHN and 1H NMR spectral data. 相似文献
992.
Shou‐Ri Sheng Xiao‐Ling Liu Yong‐Fen Tong Lie Chen Hong‐Li Wen Cai‐Sheng Song 《中国化学会会志》2005,52(5):943-946
Several new methyl substituted poly(aryl ether ketone)s containing sulfone linkage with inherent viscosities of 0.62–0.84 dL/g have been prepared from 4,4′‐bis(2‐methylphenoxy)diphenylsulfone and 4,4′‐bis(3‐methylphenoxy)diphenylsulfone with terephthaloyl chloride and isophthaloyl chloride by electrophilic Friedel‐Crafts acylation in the presence of DMF with anhydrous AlCl3 as a catalyst in 1,2‐dichloroethane, respectively. These polymers having weight‐average molecular weight in the range of 71,000–49,000 are all amorphous and show high glass transition temperatures ranging from 167 °C to 191 °C, excellent thermal stability at temperatures over 400 °C in air or nitrogen, high char yields of 51–58% in nitrogen and good solubility in CHCl3 and polar solvents such as DMF, DMSO and NMP at room temperature. 相似文献
993.
Takahiro Takayama Toshiki Mochizuki Kenichiro Todoroki Jun Zhe Min Hajime Mizuno Koichi Inoue Hiroyasu Akatsu Ichiro Noge Toshimasa Toyo'oka 《Analytica chimica acta》2015
Chiral metabolites are found in a wide variety of living organisms and some of them are understood to be physiologically active compounds and biomarkers. However, the overall analysis of chiral metabolomics is quite difficult due to the high number of metabolites, the significant diversity in their physicochemical properties, and concentration range from metabolite-to-metabolite. To solve this difficulty, we developed a novel approach for chiral metabolomics fingerprinting and chiral metabolomics extraction, which is based on the labeling of a pair of enantiomers of chiral derivatization reagents (i.e., DMT-(S,R)-Pro-OSu and DMT-3(S,R)-Apy) and precursor ion scan chromatography of the derivatives. The multivariate statistics is also required for this strategy. The proposed procedures were evaluated by the detection of a diagnostic marker (i.e., d-lactic acid) using the saliva of diabetic patients. This method was used for the determination of biomarker candidates of chiral amines and carboxyls in Alzheimer's disease (AD) brain homogenates. As the results, l-phenylalanine (L-Phe) and l-lactic acid (L-LA) were identified as the decreased and increased biomarker candidates in the AD brain, respectively. Therefore, the proposed approach seems to be helpful for the determination of non-target chiral metabolomics possessing amines and carboxyls. 相似文献
994.
First Stereoselective Synthesis of the Cytotoxic Polyketide (4R)‐1‐(3,5‐Dihydroxyphenyl)‐4‐hydroxypentan‐2‐one 下载免费PDF全文
Kothakonda Rajendra Prasad Sudina Purushotham Reddy Katragadda Suresh Babu Janaswamy Madhusudana Rao 《Helvetica chimica acta》2015,98(1):143-147
The first stereoselective synthesis of the cytotoxic polyketide (4R)‐1‐(3,5‐dihydroxyphenyl)‐4‐hydroxypentan‐2‐one ( 1 ) was achieved from readily available propylene oxide and 3,5‐dimethoxybenzyl alcohol. The synthesis involves Jacobsen's hydrolytic kinetic resolution (HKR) and Grignard reaction as key steps. 相似文献
995.
A reversed‐phase compatible thin‐layer chromatography autography for the detection of acetylcholinesterase inhibitors 下载免费PDF全文
I. Ayelen Ramallo Paula García Ricardo L. E. Furlan 《Journal of separation science》2015,38(21):3788-3794
A dual readout autographic assay to detect acetylcholinesterase inhibitors present in complex matrices adsorbed on reversed‐phase or normal‐phase thin‐layer chromatography plates is described. Enzyme gel entrapment with an amphiphilic copolymer was used for assay development. The effects of substrate and enzyme concentrations, pH, incubation time, and incubation temperature on the sensitivity and the detection limit of the assay were evaluated. Experimental design and response surface methodology were used to optimize conditions with a minimum number of experiments. The assay allowed the detection of 0.01% w/w of physostigmine in both a spiked Sonchus oleraceus L. extract chromatographed on normal phase and a spiked Pimenta racemosa (Mill.) J.W. Moore leaf essential oil chromatographed on reversed phase. Finally, the reversed‐phase thin‐layer chromatography assay was applied to reveal the presence of an inhibitor in the Cymbopogon citratus (DC.) Stapf essential oil. The developed assay is able to detect acetylcholinesterase inhibitors present in complex matrixes that were chromatographed in normal phase or reversed‐phase thin‐layer chromatography. The detection limit for physostigmine on both normal and reversed phase was of 1×10?4 μg. The results can be read by a change in color and/or a change in fluorescence. 相似文献
996.
The Synthesis of New Organoselenium Heterocyclic Compounds: 2‐aryl‐4‐phenyl‐5,6,7,8‐tetrahydro‐4H‐selenochromenes 下载免费PDF全文
Dmitriy Yurievich Direnko Yaroslav Borisovich Drevko Boris Ivanovich Drevko 《中国化学会会志》2015,62(12):1068-1071
We have explored the reactions of 2‐(3‐oxo‐1‐aryl‐3‐phenylpropyl)cyclohexanone ( 1–3 ) with hydrogen selenide in situ in conditions of acid catalysis, and synthesized new 2‐aryl‐4‐phenyl‐5,6,7,8‐tetrahydro‐4H‐selenochromenes ( 4–6 ). 相似文献
997.
Anna Grünberg Dr. Xu Yeping Dr. Hergen Breitzke Dr. Gerd Buntkowsky Prof. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(23):6993-6998
The Wilkinson’s catalyst [RhCl(PPh3)3] has been immobilized inside the pores of amine functionalized mesoporous silica material SBA‐3 and The structure of the modified silica surface and the immobilized rhodium complex was determined by a combination of different solid‐state NMR methods. The successful modification of the silica surface was confirmed by 29Si CP‐MAS NMR experiments. The presence of the Tn peaks confirms the successful functionalization of the support and shows the way of binding the organic groups to the surface of the mesopores. 31P‐31P J‐resolved 2D MAS NMR experiments were conducted in order to characterize the binding of the immobilized catalyst to the amine groups of the linkers attached to the silica surface. The pure catalyst exhibits a considerable 31P‐31P J‐coupling, well resolvable in 2D MAS NMR experiments. This J‐coupling was utilized to determine the binding mode of the catalyst to the linkers on the silica surface and the number of triphenylphosphine ligands that are replaced by coordination bonds to the amine groups. From the absence of any resolvable 31P‐31P J‐coupling in off‐magic‐angle‐spinning experiments, as well as slow‐spinning MAS experiments, it is concluded, that two triphenylphosphine ligands are replaced and that the catalyst is bonded to the silica surface through two linker molecules. 相似文献
998.
《Comptes Rendus Chimie》2015,18(10):1134-1142
Pharmaceuticals, personal care products and endocrine disruptors demonstrate huge potential to cause adverse ecological health effects at very low concentration in aquatic environment. There is a need to improve current purification technologies used in sewage and drinking-water treatment plants. This article aims at providing new insights into the recent development of natural and modified clay-based sorbents for the removal of aqueous contaminants such as pharmaceuticals and personal care products. The removal of six widely used pharmaceuticals: ibuprofen, diclofenac, ketoprofen, carbamazepine, as well as endocrine disrupting chemicals – bisphenol A and a bactericidal agent, triclosan – was examined by sorption onto eight adsorbents. Sorption was performed using natural and modified clay minerals – montmorillonite (Mt), vermiculite (VER), bentonite (B), kaolinite (K), commercial acid activated montmorillonites K10 and K30, and two carbonaceous-mineral nanocomposites, MtG5%T, BAlG3%C. This study showed that among the tested natural clays, vermiculite is the most promising sorbent for the removal of pharmaceuticals in purification processes. Among the modified clay minerals, the best results were achieved for carbonaceous bentonite and two acid activated montmorillonites K10 and K30. However, the removal of acidic pharmaceuticals on montomorillonite K10 and carbonaceous bentonite was strongly dependent on the pH value. In the case of vermiculite and acid-modified montmorillonite K30, the sorption of the selected compounds was not significantly affected by pH, which is crucial in wastewater treatment. The sorption constant divided by the specific surface area (Kd/A) is proposed to assess whether the surface area or chemical properties of the materials control the sorption process. Kd/A values were relatively high in the case of vermiculite, so it should be noticed that individual and specific surface properties of vermiculite were of crucial importance for sorption. 相似文献
999.
Daniel P. Flaherty 《Tetrahedron letters》2009,50(46):6228-10356
An efficient and widely applicable one-pot synthesis of unsymmetrical (E,E)-bis-styrylbenzenes using successive Heck and Horner-Wadsworth-Emmons reactions is described. 相似文献
1000.
阿尔茨海默病(Alzheimer’s disease,AD)是一种中枢神经系统致死性神经原发性退行病变,是老年痴呆症中最常见的一种类型.乙酰胆碱酯酶抑制剂(AChEI)是目前治疗AD的主要药物.我们选择他克林、利伐斯的明、石杉碱甲、在研药物TV-3326、多奈哌齐和Anseculin,分别与AChE进行分子对接研究.结果表明:抑制剂与AChE结合能力的大小顺序为:他克林〈利伐斯的明〈石杉碱甲〈TV.3326〈多奈哌齐〈Anseculin,这与实验中测得ACHE1的IC50值反应活性大小一致.上述6类药物分子,Anseculin与AChE的相互作用能力最强. 相似文献