Recyclable N-heterocyclic carbene/palladium catalyst on graphene oxide for the aqueous-phase Suzuki reaction

Graphene oxide (GO) was functionalized with a N-heterocyclic carbene (NHC) precursor, 3-(3-aminopropyl)-1-methylimidazolium bromide ([APMIm][Br]) for the immobilization of palladium catalyst. The GO-supported NHC precursor (IMGO) formed a stable complex with Pd(OAc)₂ (GO–NHC–Pd), which showed excellent catalytic activity and fast reaction kinetics in the aqueous-phase Suzuki reaction of aryl bromides and chlorides at relatively mild conditions (1 h at 50 °C). The GO–NHC–Pd catalyst was reused several times without any loss of its catalytic activity in the Suzuki reaction of aryl bromide.     

Precise characterization method of antibody‐conjugated magnetic nanoparticles for pathogen detection using stuffer‐free multiplex ligation‐dependent probe amplification

Antibody‐conjugated magnetic nanoparticles (Ab‐MNPs) have potential in pathogen detection because they allow target cells to be easily separated from complex sample matrices. However, the sensitivity and specificity of pathogen capture by Ab‐MNPs generally vary according to the types of MNPs, antibodies, and sample matrices, as well as preparation methods, including immobilization. Therefore, achieving a reproducible analysis utilizing Ab‐MNPs as a pathogen detection method requires accurate characterization of Ab‐MNP capture ability and standardization of all handling processes. In this study, we used high‐resolution CE‐single strand conformational polymorphism coupled with a stuffer‐free multiplex ligation‐dependent probe amplification system to characterize Ab‐MNPs. The capture ability of Ab‐MNPs targeting Salmonella enteritidis and nine pathogens, including S. enteritidis, was analyzed in phosphate buffer and milk. The effect of storage conditions on the stability of Ab‐MNPs was also assessed. The results showed that the stuffer‐free multiplex ligation‐dependent probe amplification system has the potential to serve as a standard characterization method for Ab‐MNPs. Moreover, the precise characterization of Ab‐MNPs facilitated robust pathogen detection in various applications.     

Synthesis of novel 2,4,6,8,10-pentaaza[3.3.3]propellane derivatives

Propellanes and azapropellanes are attractive compounds for their unique structure and valuable applications but there are few synthetic studies for highly N-substituted azapropellanes. Several novel derivatives of 2,4,6,8,10-pentaaza[3.3.3]propellane, such as 3, 4, and 5 were successfully synthesized from readily available diethyl tartrate. Most of the synthetic steps were efficient. Their propellane structures were established by spectroscopic data and confirmed with single crystal X-ray analyses.     

Preparation of 2,2-difluoro-1-trialkylsilylethenylstannanes and their cross-coupling reactions

Reaction of 2 with bis(tributyltin) in the presence of 3 mol % Pd₂(dba)₃, 6 mol % XPhos, and 30 equiv of LiBr in wet and air bubbled THF at reflux for 8 h afforded the desired products 3 in 73–74% yields. The cross-coupling reaction of 3a with aryl iodides in the presence of 10 mol % Pd(PPh₃)₄ and 10 mol % CuI afforded the coupled products 4a–p in 47–90% yields. The coupling reaction of 3b with various alkynyl bromides having aryl-, alkyl, or trialkylsilyl group also afforded the corresponding 1,3-enynes 5a–g in 61–77% yields.     

Nucleophile‐Dependent Regio‐ and Stereoselective Ring Opening of 1‐Azoniabicyclo[3.1.0]hexane Tosylate

1‐[(1R)‐(1‐Phenylethyl)]‐1‐azoniabicyclo[3.1.0]hexane tosylate was generated as a stable bicyclic aziridinium salt from the corresponding 2‐(3‐hydroxypropyl)aziridine upon reaction with p‐toluenesulfonyl anhydride. This bicyclic aziridinium ion was then treated with various nucleophiles including halides, azide, acetate, and cyanide in CH₃CN to afford either piperidines or pyrrolidines through regio‐ and stereoselective ring opening, mediated by the characteristics of the applied nucleophile. On the basis of DFT calculations, ring‐opening reactions under thermodynamic control yield piperidines, whereas reactions under kinetic control can yield both piperidines and pyrrolidines depending on the activation energies for both pathways.     

Efficient Diketopyrrolopyrrole‐Based Small‐Molecule Bulk‐Heterojunction Solar Cells with Different Electron‐Donating End‐Groups

A series of small molecules that contained identical π‐spacers (ethyne), a central diketopyrrolopyrrole (DPP) unit, and different aromatic electron‐donating end‐groups were synthesized and used in organic solar cells (OSCs) to study the effect of electron‐donating groups on the device performance. The three compounds, DPP‐A‐Ph , DPP‐A‐Na , and DPP‐A‐An , possessed intense absorption bands that covered a wide range, from 350 to 750 nm, and relatively low HOMO energy levels, from ?5.50 to ?5.55 eV. DPP‐A‐An , which contained anthracene end‐groups, demonstrated a stronger absorbance and a higher hole mobility than DPP‐A‐Ph , which contained phenyl groups, and DPP‐A‐Na , which contained naphthalene units. The power‐conversion efficiencies (PCEs) of OSCs based on organic:PC₇₁BM blends (1:1, w/w) with a processed DIO additive were 3.93 % for DPP‐A‐An , 3.02 % for DPP‐Na , and 2.26 % for DPP‐A‐Ph . These findings suggest that a DPP core that is functionalized with electron‐donating capping groups constitutes a promising new class of solution‐processable small molecules for OSC applications.     

A study on solidification of CaCO3 powder containing C-14 by using a low melting glass material

Journal of Radioanalytical and Nuclear Chemistry - CaCO3 powder containing C-14, which has a long half-life, is generated from the treatment process of spent activated carbons from the air cleaning...     

Review on the thickness measurement of ultrathin oxide films by mutual calibration method

Mutual calibration was suggested as a method to determine the absolute thickness of ultrathin oxide films. It was motivated from the large offset values in the reported thicknesses in the Consultative Committee for Amount of Substance (CCQM) pilot study P-38 for the thickness measurement of SiO₂ films on Si(100) and Si(111) substrates in 2004. Large offset values from 0.5 to 1.0 nm were reported in the thicknesses by ellipsometry, X-ray reflectometry (XRR), medium-energy ion scattering spectrometry (MEIS), Rutherford backscattering spectroscopy (RBS), nuclear reaction analysis (NRA), and transmission electron microscopy (TEM). However, the offset value for the thicknesses by X-ray photoelectron spectroscopy (XPS) was close to zero (−0.013 nm). From these results, the mutual calibration method was reported for the thickness measurement of SiO₂ films on Si(100) by combination of TEM and XPS. The mutual calibration method has been applied for the thickness measurements of hetero oxide films such as Al₂O₃ and HfO₂. Recently, the effect of surface contamination was reported to be critical to the thickness measurement of HfO₂ films by XPS. On the other hand, MEIS was proved to be a powerful zero offset method which is not affected by the surface contamination. As a result, the reference thicknesses in the CCQM pilot study P-190 for the thickness measurement of HfO₂ films on Si(100) substrate were determined by mutual calibration method from the average XRR data and MEIS analysis. Conclusively, the thicknesses of ultrathin oxide films can be traceably certified by mutual calibration method and most thickness measurement methods can be calibrated from the certified thicknesses.     

Single-drop microextraction technique for the determination of antibiotics in environmental water

Growing concerns related to antibiotic residues in environmental water have encouraged the development of rapid, sensitive, and accurate analytical methods. Single-drop microextraction has been recognized as an efficient approach for the isolation and preconcentration of several analytes from a complex sample matrix. Thus, single-drop microextraction techniques are cost-effective and less harmful to the environment, subscribing to green analytical chemistry principles. Herein, an overview and the current advances in single-drop microextraction for the determination of antibiotics in environmental water are presented were included. In particular, two main approaches used to perform single-drop microextraction (direct immersion-single-drop microextraction and headspace-single-drop microextraction) are reviewed. Furthermore, the impressive analytical features and future perspectives of single-drop microextraction are discussed in this review.     

Process Development for the Detoxification of Fermentation Inhibitors from Acid Pretreated Microalgae Hydrolysate

The aim of this study was to remove 5-hydroxymethyl furfural (5-HMF) and furfural, known as fermentation inhibitors, in acid pretreated hydrolysates (APH) obtained from Scenedesmus obliquus using activated carbon. Microwave-assisted pretreatment was used to produce APH containing glucose, xylose, and fermentation inhibitors (5-HMF, furfural). The response surface methodology was applied to optimize key detoxification variables such as temperature (16.5–58.5 °C), time (0.5–5.5 h), and solid–liquid (S-L) ratio of activated carbon (0.6–7.4 w/v%). Three variables showed significant effects on the removal of fermentation inhibitors. The optimum detoxification conditions with the maximum removal of fermentation inhibitors and the minimum loss of sugars (glucose and xylose) were as follows: temperature of 36.6 °C, extraction time of 3.86 h, and S-L ratio of 3.3 w/v%. Under these conditions, removal of 5-HMF, furfural, and sugars were 71.6, 83.1, and 2.44%, respectively, which agreed closely with the predicted values. When the APH and detoxified APH were used for ethanol fermentation by S. cerevisiae, the ethanol produced was 38.5% and 84.5% of the theoretical yields, respectively, which confirmed that detoxification using activated carbon was effective in removing fermentation inhibitors and increasing fermentation yield without significant removal of fermentable sugars.