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Preparation and Regioselective Metalation of Bis(trimethylsilyl)methyl‐Substituted Aryl Derivatives 下载免费PDF全文
Veronika Werner Thomas Klatt Masaya Fujii Jenifer Markiewicz Prof. Dr. Yitzhak Apeloig Prof. Dr. Paul Knochel 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(27):8338-8342
A range of bis(trimethylsilyl)methyl‐substituted aryl derivatives was prepared by using a Kumada–Corriu cross‐coupling reaction. The regioselective metalation of the resulting bis(trimethylsilyl)methyl‐substituted aryl derivatives bearing this bulky silyl group allowed the generation of functionalized aromatics. A regioselective switch in the presence or in the absence of the bis(trimethylsilyl)methyl group has been demonstrated. Furthermore, this silyl group was converted into a formyl group or a styryl group, enhancing the scope of application of such bis(trimethylsilyl)methyl‐substituted arenes. 相似文献
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Gabla Jenifer J. Lathiya Dharmesh R. Revawala Akash A. Maheria Kalpana C. 《Research on Chemical Intermediates》2019,45(4):1863-1881
Research on Chemical Intermediates - Propylsulfonic acid functionalized Santa Barbara Amorphous-15 (SBA-15–Pr–SO3H) catalyst has been synthesized using a surface modification of... 相似文献
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T.A. Jenifer Vijay Kebbahalli N. NandeeshGoravanahalli M. Raghavendra Kanchugarakoppal S. RangappaKempegowda Mantelingu 《Tetrahedron letters》2013
A convenient one-pot method for the synthesis of thiochromen-4-ones by the condensation of 2′-haloacetophenone and dithioesters at room temperature in the presence of NaH in DMF in moderate to good yields has been developed. The method involves unusual intramolecular S-arylation. The reaction is operationally facile, readily scalable and offers rapid entry into substituted chromene-4-ones. 相似文献
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The synthesis of a family of Gemini Amphiphilic Pseudopeptide (GAP) molecules by a reductive amination reaction has been carried out. The process is highly modular and can be efficiently performed with different pseudopeptidic diamines as well as aliphatic and aromatic aldehydes. Preliminary studies showed the abilities of the GAPs to self-assemble into supramolecular nanostructures. 相似文献
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Péres VF Saffi J Melecchi MI Abad FC de Assis Jacques R Martinez MM Oliveira EC Caramão EB 《Journal of chromatography. A》2006,1105(1-2):115-118
This paper describes a comparative study of extraction methods of terpenes (terpenic alcohols and phytosterols), fatty acids and Vitamin E from leaves of Piper gaudichaudianum Kunth. The analysis of extracts was done by gas chromatography with mass spectrometric detection. The identification and quantification was made by co-injections of the extract with certified standards. The use of pressurized liquid extraction (PLE; Dionex trade name: ASE, for accelerated solvent extraction) decrease significantly the total time of extraction, the amount of solvent and the manipulation of sample and solvents in comparison with soxhlet (SE) and ultrasound-assisted (USE). In addition, PLE was more effective for the extractions of terpenes (terpenic alcohols and phytosterols), fatty acids and Vitamin E. 相似文献
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Bardin S Guo W Johnson JL Khan S Ahmad A Duggan JX Ayoub J Ahmad I 《Journal of chromatography. A》2005,1073(1-2):249-255
A simple, rapid and sensitive LC-MS/MS bioanalytical method has been developed to simultaneously quantify Camptosar (CPT-11) and its active metabolite, SN-38, in mouse plasma and tissues. A single step protein precipitation with acetonitrile in 96-well plates was used for sample preparation. Camptothecin (CPT) was used as the internal standard. Fast separation of SN-38, CPT-11 and CPT was carried out isocratically on a C18, 2 mm x 50 mm, 5 microm HPLC column with a mobile phase containing acetonitrile and 20 mM ammonium acetate (pH 3.5) and a 2.5 min chromatographic run time. The API 4000 MS/MS system was operated in positive ionization multiple reaction monitoring mode, and the transitions for SN-38, CPT-11 and CPT were 393.4 --> 349.3, 587.6 --> 167.2 and 349.3 --> 305.3, respectively. The SN-38 and CPT-11 concentrations in samples were calculated from a standard curve of peak area ratios of the analyte to that of the internal standard using a 1/chi2 weighted linear regression. The quantitation limit of 0.5 ng/mL was achieved by using a low sample volume (100 microL) of plasma or tissue homogenates. The assay was linear over the concentration range of 0.5-500 ng/mL with acceptable precision and accuracy. The method was used for the quantification of CPT-11 and SN-38 in plasma and tissues to support a preclinical pharmacokinetics and tissue distribution study of CPT-11 in mice. 相似文献
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Alfonso I Bolte M Bru M Burguete MI Luis SV Rubio J 《Journal of the American Chemical Society》2008,130(19):6137-6144
The anion-templated synthesis of different pseudopeptidic macrocycles has been studied in detail by using a multidisciplinary approach. The reaction between an open-chain pseudopeptidic diamine and the appropriate dialdehyde is highly affected by the presence of the best fitting anionic template. The formation of the corresponding macrocyclic tetraimino-template supramolecular complex is demonstrated by NMR (ROESY and PGSE) and mass spectrometry (ESI-TOF). These supramolecular complexes can be easily reduced to the corresponding more stable tetraamine macrocycles. Accordingly, we have used this reaction to efficiently synthesize a family of new pseudopeptidic macrocycles in a one-pot two-steps anion-templated reductive amination reaction, which comprises a multicomponent macrocyclization through the selective formation of four chemical bonds to yield a unique macrocyclic structure. Different variables like the aliphatic spacer between amino acidic moieties, geometry of the dialdehyde, and structure of the amino acid side chains were thoroughly studied, and their effect in the formation and stability of the supramolecular complexes discussed. The conformational preorganization induced by the template has been monitored by circular dichroism, reflecting the differences observed in the isolated yields, as well as by NMR spectroscopy. This effect has been also supported by molecular modeling. All the experimental and theoretical techniques were strongly consistent and reflected the same trends by comparing the different structural variables introduced in the system. 相似文献
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Dr. Jenifer Pendiuk Gonçalves Duangkamol Promlok Tsvetomir Ivanov Shijia Tao Timo Rheinberger Seong-Min Jo Yingjie Yu Robert Graf Manfred Wagner Assoc. Prof. Daniel Crespy Frederik R. Wurm Dr. Lucas Caire da Silva Prof. Shuai Jiang Prof. Katharina Landfester 《Angewandte Chemie (International ed. in English)》2023,62(11):e202216966
Living organisms compartmentalize their catalytic reactions in membranes for increased efficiency and selectivity. To mimic the organelles of eukaryotic cells, we develop a mild approach for in situ encapsulating enzymes in aqueous-core silica nanocapsules. In order to confine the sol-gel reaction at the water/oil interface of miniemulsion, we introduce an aminosilane to the silica precursors, which serves as both catalyst and an amphiphilic anchor that electrostatically assembles with negatively charged hydrolyzed alkoxysilanes at the interface. The semi-permeable shell protects enzymes from proteolytic attack, and allows the transport of reactants and products. The enzyme-carrying nanocapsules, as synthetic nano-organelles, are able to perform cascade reactions when enveloped in a polymer vesicle, mimicking the hierarchically compartmentalized reactions in eukaryotic cells. This in situ encapsulation approach provides a versatile platform for the delivery of biomacromolecules. 相似文献