Ultrasound accelerated Claisen-Schmidt condensation: A green route to chalcones

Chalcones have been synthesized under sonochemical irradiation by Claisen-Schmidt condensation between benzaldehyde and acetophenone. Two basic activated carbons (Na and Cs-Norit) have been used as catalysts. The effect of the ultrasound activation has been studied. A substantial enhancing effect in the yield was observed when the carbon catalyst was activated under ultrasonic waves. This “green” method (combination of alkaline-doped carbon catalyst and ultrasound waves) has been applied to the synthesis of several chalcones with antibacterial properties achieving, in all cases, excellent activities and selectivities. A comparative study under non-sonic activation has showed that the yields are lower in silent conditions, indicating that the sonication exerts a positive effect on the activity of the catalyst. Cs-doped carbon is presented as the optimum catalyst, giving excellent activity for this type of condensation. Cs-Norit carbon catalyst can compete with the traditional NaOH/EtOH when the reaction is carried out under ultrasounds. The role of solvent in this reaction was studied with ethanol. High conversion was obtained in absence of solvent. The carbons were characterized by thermal analysis, nitrogen adsorption and X-ray photoelectron spectroscopy.     

Optimization of STEM-HAADF Electron Tomography Reconstructions by Parameter Selection in Compressed Sensing Total Variation Minimization-Based Algorithms

A novel procedure to optimize the 3D morphological characterization of nanomaterials by means of high angle annular dark field scanning-transmission electron tomography is reported and is successfully applied to the analysis of a metal- and halogen-free ordered mesoporous carbon material. The new method is based on a selection of the two parameters (μ and β) which are key in the reconstruction of tomographic series by means of total variation minimization (TVM). The parameter-selected TVM reconstructions obtained using this approach clearly reveal the porous structure of the carbon-based material as consisting of a network of parallel, straight channels of ≈6 nm diameter ordered in a honeycomb-type arrangement. Such an unusual structure cannot be retrieved from a TVM 3D reconstruction using default reconstruction values. Moreover, segmentation and further quantification of the optimized 3D tomographic reconstruction provide values for different textural parameters, such as pore size distribution and specific pore volume that match very closely with those determined by macroscopic physisorption techniques. The approach developed can be extended to other reconstruction models in which the final result is influenced by parameter choice.     

Synthesis of Densely Packaged,Ultrasmall Pt02 Clusters within a Thioether‐Functionalized MOF: Catalytic Activity in Industrial Reactions at Low Temperature

The gram‐scale synthesis, stabilization, and characterization of well‐defined ultrasmall subnanometric catalytic clusters on solids is a challenge. The chemical synthesis and X‐ray snapshots of Pt⁰₂ clusters, homogenously distributed and densely packaged within the channels of a metal–organic framework, is presented. This hybrid material catalyzes efficiently, and even more importantly from an economic and environmental viewpoint, at low temperature (25 to 140 °C), energetically costly industrial reactions in the gas phase such as HCN production, CO₂ methanation, and alkene hydrogenations. These results open the way for the design of precisely defined catalytically active ultrasmall metal clusters in solids for technically easier, cheaper, and dramatically less‐dangerous industrial reactions.     

In situ transmission electron microscopy investigation of Ce(IV) and Pr(IV) reducibility in a Rh (1%)/Ce0.8Pr0.2O(2-x) catalyst

In-situ Atomic Resolution Transmission Electron Microscopy studies carried out on a Rh/Ce0.8Pr0.2O(2-x) catalyst, under hydrogen in the temperature range 298-1223 K, show the occurrence of consecutive reduction of Pr4+ and Ce4+ ions, and the formation of an oxygen-deficient Ln16O30 (Ln: Ce, Pr) ordered phase.     

Magnetic nanoparticles--templated assembly of protein subunits: a new platform for carbohydrate-based MRI nanoprobes

A new approach for the preparation of carbohydrate-coated magnetic nanoparticles is reported. In a first step, we show that the pH-driven assembly-disassembly natural process that occurs in apoferritin protein is effective for the encapsulation of maghemite nanoparticles of different sizes: 4 and 6 nm. In a second step, we demonstrate that the presence of functional amine groups in the outer shell of apoferritin allows functionalization with two carbohydrates, N-acetyl-D-glucosamine and d-mannose. High-resolution electron microscopy (HREM), high angle annular dark field scanning electron microscopy (HAADF-STEM), electron energy loss spectroscopy (EELS), X-ray diffraction (XRD), and SQUID technique have been used to characterize the magnetic samples, termed herein Apomaghemites. The in vivo magnetic resonance imaging (MRI) studies showed the efficiency in contrasting images for these samples; that is, the r(2) NMR relaxivities are comparable with Endorem (a commercial superparamagnetic MRI contrast agent). The r(2) relaxivity values as well as the pre-contrast and post-contrast T(2)*-weighted images suggested that our systems could be used as perspective superparamagnetic contrast agents for magnetic resonance imaging (MRI). The carbohydrate-functionalized Apomaghemite nanoparticles retained their recognition abilities, as demonstrated by the strong affinity with their corresponding carbohydrate-binding lectins.     

Unsymmetrically substituted furoxans. VIII. Chloromethylfuroxans

The two isomeric chloromethylfuroxans have been prepared. Their structures, thermal equilibration and reaction toward thiophenoxide ion are discussed. Kinetics of the 4-methyl — 3-methyl isomer thermal conversion are also reported.     

Gold nanoparticles in organic capsules: a supramolecular assembly of gold nanoparticles and cucurbituril

Gold nanoparticles (相似文献