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51.
Biology‐Oriented Synthesis of a Withanolide‐Inspired Compound Collection Reveals Novel Modulators of Hedgehog Signaling 下载免费PDF全文
Dr. Jakub Švenda Dipl.‐Biochem. Michael Sheremet M. Sc. Lea Kremer Lukáš Maier Dr. Jonathan O. Bauer Prof. Dr. Carsten Strohmann Dr. Slava Ziegler Dr. Kamal Kumar Prof. Dr. Herbert Waldmann 《Angewandte Chemie (International ed. in English)》2015,54(19):5596-5602
Biology‐oriented synthesis employs the structural information encoded in complex natural products to guide the synthesis of compound collections enriched in bioactivity. The trans‐hydrindane dehydro‐δ‐lactone motif defines the characteristic scaffold of the steroid‐like withanolides, a plant‐derived natural product class with a diverse pattern of bioactivity. A withanolide‐inspired compound collection was synthesized by making use of three key intermediates that contain this characteristic framework derivatized with different reactive functional groups. Biological evaluation of the compound collection in cell‐based assays that monitored biological signal‐transduction processes revealed a novel class of Hedgehog signaling inhibitors that target the protein Smoothened. 相似文献
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We report a new in-tube solid phase microextraction approach named electrochemically controlled in-tube solid phase microextraction (EC in-tube SPME). This approach, which combined electrochemistry and in-tube SPME, led to decrease in total analysis time and increase in sensitivity. At first, pyrrole was elctropolymerized on the inner surface of a stainless steel tube. Then, the polypyrrole (PPy)-coated in-tube SPME was coupled on-line to liquid chromatography (HPLC) to achieve automated in-tube SPME–HPLC analysis. After the completion of EC-in-tube SPME–HPLC setup, the PPy-coated tube was used as working electrode for uptake of diclofenac as target analyte. Extraction ability of the tube in presence and in absence of applied electrical field was investigated. It was found that, under the same extraction conditions, the extraction efficiency could be greatly enhanced by using the constant potential. Important factors are also optimized. The detection limit (S/N = 3) and precision were 0.1 μg L−1 and 4.4%, respectively. 相似文献
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In-tube magnetic solid phase microextraction (in-tube MSPME) of fluoroquinolones from water and urine samples based on the use of sodium dodecyl sulfate (SDS) coated Fe3O4 nanoparticles packed tube has been reported. After the preparation of Fe3O4 nanoparticles (NPs) by a batch synthesis, these NPs were introduced into a stainless steel tube by a syringe and then a strong magnet was placed around the tube, so that the Fe3O4 NPs were remained in the tube and the tube was used in the in-tube SPME-HPLC/UV for the analysis of fluoroquinolones in water and urine samples. Plackett–Burman design was employed for screening the variables significantly affecting the extraction efficiency. Then, the significant factors were more investigated by Box–Behnken design. Calibration curves were linear (R2 > 0.990) in the range of 0.1–1000 μg L−1 for ciprofloxacin (CIP) and 0.5–500 μg L−1 for enrofloxacin (ENR) and ofloxacin (OFL), respectively. LODs for all studied fluoroquinolones ranged from 0.01 to 0.05 μg L−1. The main advantages of this method were rapid and easy automation and analysis, short extraction time, high sensitivity, possibility of fully sorbent collection after analysis, wide linear range and no need to organic solvents in extraction. 相似文献
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A New and Facile Synthesis of Novel Pyrazolothienopyrimidines and Imidazopyrazolothienopyrimidines 下载免费PDF全文
4‐Amino‐3‐methyl‐1‐phenyl‐1H‐thieno[2,3‐c]pyrazole‐5‐carboxamide ( 5 ), which was synthesized by an innovative method, was used as a versatile precursor for synthesizing pyrazolothienopyrimidines and imidazopyrazolothienopyrimidines compounds. Reaction of amino thienopyrazole carboxamide 5 with triethyl orthoformate afforded thienopyrazolopyrimidine 6 . Chlorination of the latter compound, using phosphorus oxychloride afforded the chloro pyrazolothienopyrimidine 7 , which underwent nucleophilic substitution reactions with various primary and secondary amines to give the alkyl (aryl) amino pyrimidine compounds 8a–d . On the other hand, the reaction of chloropyrimidine 7 with thiourea afforded the pyrimidine thione compound 9 , which was alkylated with α‐halogentaed compounds to afford the S‐alkylated derivatives 10a–c . Also, chloroacetylation of the amino carboxamide 5 using chloroacetyl chloride yielded the chloromethyl pyrazolothienopyrimidine 12 , which underwent nucleophilic substitu‐ tion reactions with various primary and secondary amines to afford the alkyl (aryl) aminomethyl compounds 13a–f . The latter Compounds underwent Mannich reaction to give imidazopyrimidothieno‐ pyrazoles 14a–c . The newly synthesized compounds and their derivatives were fully characterized by elemental and spectral analysis. 相似文献
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Exploiting the 1,2,3‐Triazole Moiety to Generate Carbazole Molecular Architectures through Click Approach 下载免费PDF全文
Mohamed A. Ameen Kamal M. El‐Shaieb Asmaa H. Mohamed Fathy F. Abdel‐Latif 《Journal of heterocyclic chemistry》2015,52(6):1718-1722
Reaction of 3,6‐dichlorocarbazole with propargyl bromide in the presence of a basic medium gave an N‐propargylated carbazole. The latter compound was converted into molecular architectures containing 1,2,3‐triazole moiety through Cu(I)‐catalyzed 1,3‐cycloaddition reaction with different azides. Similarly, 2‐azidomethyl benzothiazole was cliched with N‐Boc‐protected N´‐propargyl glutamate to give the biomolecule 2‐triazolylmethyl product. 相似文献
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