Search Results (8)

We developed a new optical sensor for tracing Hg(II) ions. The detection affinity examines within a concentration range of 0–4.0 µM Hg(II). The sensor film is based on Methyl 2-hydroxy-3-(((2S,2’R,3a’S,5R)-2-isopropyl-5,5’-dimethyl-4’-oxotetrahydro-2’H-spiro[cy-clohexane-1,6’-im-idazo[1,5-b]isoxazol]-2’-yl)methyl)-5-methylbenzoate (IXZD). The novel synthesized compound could be utilized as an optical turn-on chemosensor for pH. The emission intensity is highly enhanced for the deprotonated form concerning the protonated form. IXZD probe has a characteristic fluorescence peak at 481 nm under excitation of 351 nm with large Stocks shift of approximately 130 nm. In addition, the binding process of IXZD:Hg(II) presents a 1:1 molar ratio which is proved by the large quench of the 481 nm emission peak of IXZD and the growth of a new emission peak at 399 nm (blue shift). The binding configurations with one Hg(II) cation and its electronic characteristics were investigated by applying the Density Functional Theory (DFT) and the time-dependent DFT (TDDFT) calculations. Density functional theory (DFT) and the time-dependent DFT (TDDFT) theoretical results were provided to examine Hg(II)-IXZD structures and their electronic properties in solution. The developed chemical sensor was offered based on the intramolecular charge transfer (ICT) mechanism. The sensor film has a significantly low limit of detection (LOD) for Hg(II) of 0.025 μM in pH 7.4, with a relative standard deviation RSD_r (1%, n = 3). Lastly, the IXZD shows effective binding affinity to mercury ions, and the binding constant K_b was estimated to be 5.80 × 10⁵ M⁻¹. Hence, this developed optical sensor film has a significant efficiency for tracing mercury ions based on IXZD molecule-doped sensor film. Full article

Herein, we report a bisoxazole derivative as well as a bromo-substituted oxazole derivatives via a simple approach. The synthesis begins with an inexpensive and readily available starting material, such as 2,5-dimethoxybenzaldehyde, hydroquinone, and p-toluenesulfonylmethyl isocyanide (TosMIC). This approach relies on the Van Leusen oxazole method and electrophilic aromatic bromination. The structures of bisoxazole and bromosubstituted aryloxazoles were fully supported by spectroscopic methods (IR, NMR, and HRMS) and further established using single crystal X-ray diffraction studies. Full article

Fabric-reinforced cementitious matrix (FRCM) composites, comprising high-strength fiber textiles embedded within inorganic matrices, represent an effective, cost-efficient, and low-invasive solution for strengthening and retrofitting existing masonry and reinforced concrete structures. Among different textiles employed in FRCM composites, polyparaphenylene benzo-bisoxazole (PBO) textiles are adopted due to their high tensile strength and good adhesion with the matrix. Although several experimental, numerical, and analytical works were performed to investigate the mechanical properties of PBO FRCM composites, limited information is available on their long-term behavior, as well as in the case of exposure to aggressive environments. This paper presents and discusses the results of a wide experimental campaign aimed at investigating the effect of different environmental conditions on the long-term tensile behavior of a PBO FRCM composite. Tests are performed using a clamping-grip tensile test set-up. The effect of various aggressive environments on the composite matrix cracking stress, composite tensile strength, ultimate strain, and fully cracked stage slope is investigated by comparing the results of nominally equal conditioned and unconditioned (control) specimens. These results are also compared with those of other FRCM composites comprising glass and carbon textiles subjected to the same conditionings, collected from the literature. The results show only limited reductions in the tensile properties, even after long exposure to aggressive environments. Full article

Activation of a hydroxyl group towards nucleophilic substitution via reaction with methanesulfonyl chloride or PPh₃-CBr₄ system is a commonly used pathway to various functional derivatives. The reactions of (5R(S),6R(S))-1-X-6-(hydroxymethyl)-2,2-dimethyl- 1-azaspiro[4.4]nonanes 1a–d (X = O·; H; OBn, OBz) with MsCl/NR₃ or PPh₃-CBr₄ were studied. Depending on substituent X, the reaction afforded hexahydro-1H,6H-cyclopenta[c]pyrrolo[1,2-b]isoxazole (2) (for X = O), a mixture of 2 and octahydrocyclopenta[c]azepines (4–6) (for X = OBn, OBz), or perhydro-cyclopenta[2,3]azeto[1,2-a]pyrrol (3) (for X = H) derivatives. Alkylation of the latter with MeI with subsequent Hofmann elimination afforded 2,3,3-trimethyl-1,2,3,4,5,7,8,8a-octahydrocyclopenta[c]azepine with 56% yield. Full article

In recent decades, bicyclic nitroxyl radicals have caught chemists’ attention as selective catalysts for the oxidation of alcohols and amines and as additives and mediators in directed C-H oxidative transformations. In this regard, the design and development of synthetic approaches to new functional bicyclic nitroxides is a relevant and important issue. It has been reported that imidazo[1,2-b]isoxazoles formed during the condensation of acetylacetone with 2-hydroxyaminooximes having a secondary hydroxyamino group are recyclized under mild basic catalyzed conditions to 8-hydroxy-5-methyl-3-oxo-6,8-diazabicyclo[3.2.1]-6-octenes. The latter, containing a sterically hindered cyclic N-hydroxy group, upon oxidation with lead dioxide in acetone, virtually quantitatively form stable nitroxyl bicyclic radicals of a new class, which are derivatives of both 2,2,6,6-tetramethyl-4-oxopiperidine-1-oxyl (TEMPON) and 3-imidazolines. Full article

Several reinforced-concrete (RC) structural elements are subjected to cyclic load, such those employed in highway and railroad bridges and viaducts. The durability of these elements may be reduced as a consequence of fatigue, which mainly affects the steel reinforcement. The use of externally bonded (EB) fiber-reinforced cementitious matrix (FRCM) composites allows the moment capacity to be shared by the internal reinforcement and the EB composite, thus increasing the fatigue life of the strengthened RC member. The effectiveness of EB FRCM composites is related to the composite bond properties. However, limited research is currently available on the effect of fatigue on the bond behavior of FRCM-substrate joints. This study provides first the state of the art on the fatigue behavior of different FRCM composites bonded to a concrete substrate. Then, the fatigue bond behavior of a polyparaphenylene benzo-bisoxazole (PBO) FRCM is experimentally investigated using a modified beam test set-up. The use of this set-up provided information on the effect of fiber-matrix interface shear and normal stresses on the specimen fatigue bond behavior. The results showed that fatigue loading may induce premature debonding at the matrix-fiber interface and that stresses normal to the interface reduce the specimen fatigue life. Full article

The behavior of FRCM (Fabric Reinforced Cementitious Mortar) confined clay brick masonry columns is analyzed in this paper. The results of an experimental investigation conducted on small-scale columns made by clay brick masonry confined with steel-FRCM (or Steel Reinforced Grout, SRG), PBO (poly-paraphenylene-benzo-bisoxazole) FRCM and basalt-FRCM, tested under monotonic compressive load, are described and discussed. Tests were conducted on thirteen prismatic columns; eleven columns (two unconfined and nine confined) were tested under concentric load while an eccentric load was applied on two confined columns. For each confinement system, the parameters investigated were the ‘confinement ratio’, the ‘load eccentricity’ and the ‘overlap configuration of the fiber fabrics’. FRCM confinement improved the structural response of masonry columns in terms of ultimate strength, ultimate strain and ductility. Some models from the literature were also examined to evaluate their applicability in predicting the axial capacity of confined columns. Full article