Organic-salt-mediated highly regioselective N3-alkylation of 2-thiophenytoin via Michael reaction under solvent-free conditions

A regioselective N3-alkylation of 5,5-diphenyl-2-thiohydantoin (2-thiophenytoin) using a very efficient mild base K₂CO₃ and α,β-unsaturated esters in the presence of organic salt TBAB (tetrabutylammonium bromide) at room temperature has been reported (3b–3h). The selectivity of this reaction is excellent and products have been produced in good yields under solvent-free conditions. The increase of the reaction temperature to 70°C mostly disappeared this selectivity and afforded only the N1,N3-dialkylated derivatives of 2-thiophenytoin in good yields (4b–4g). We were unable to selectively N3-alkylate 2-thiophenytoin with ethyl acrylate at both room temperature and 70°C under the same conditions (4a). Dimethyl and diethyl fumarates cannot work as Michael acceptors and were hydrolyzed to fumaric acid under reaction conditions.     

Experimental study and nuclear model calculation for 65Zn production

Excitation functions and theoretical yields via charge particle induced reactions were evaluated using EMPIRE-3.2.2 and ALICE/ASH codes and the obtained results have been discussed and compared with the available reported experimental data. It has been verified that ^natCu(p,n)⁶⁵Zn reaction is the optimum ⁶⁵Zn production route. The ⁶⁵Zn was produced using ^natCu(p,xn) ⁶⁵Zn reaction in the energy range of 16.8 → 12.2 MeV with the thick target yield of 0.15 ± 0.005 MBq/μA h. The ⁶⁵Zn radionuclide was purified by anion exchange chromatography.

     

Stability evaluation of tramadol enantiomers using a chiral stability-indicating capillary electrophoresis method and its application to pharmaceutical analysis

In this study, a chiral stability-indicating CE assay was developed for the stability evaluation of tramadol (TR) enantiomers in commercial tablets using maltodextrin as chiral selector. To investigate the stability-indicating power of the analytical method as well as stability evaluation of TR enantiomers, active pharmaceutical ingredient and TR tablets were subjected to photolysis, heat, oxidation and hydrolysis to conduct stress testing. Best separation for the TR enantiomers was achieved on an uncoated fused-silica capillary at 20 °C using borate buffer (50 mM, pH 10.2) containing 10% m/v maltodextrin. All determinations were performed by a UV detector at 214 nm. A constant voltage of 20 kV was applied to obtain the separation. The range of quantitation for both enantiomers was 5-100 μg/mL (R>0.996). Intra- and inter-day RSD (n=6) were less than 10%. The percent relevant errors were obtained to be less than 4.0 for both enantiomers. The limits of quantitation and detection for both enantiomers were 5 and 1.5 μg/mL, respectively. Degradation products resulting from the stress studies were the same for both enantiomers and did not interfere with the detection of the enantiomers.     

Rapid and Highly Sensitive Detection of Target DNA Related to COVID-19 Virus With a Fluorescent Bio-conjugated Probe via a FRET Mechanism

Journal of Fluorescence - A novel cyanine 3 (Cy3)-based bio-conjugated sensor has been developed to detect target DNA or extracted RNA from COVID -19 samples using the fluorescence resonance energy...     

Face-spiral codes in cubic polyhedral graphs with face sizes no larger than 6

According to the face-spiral conjecture, first made in connection with enumeration of fullerenes, a cubic polyhedron can be reconstructed from a face sequence starting from the first face and adding faces sequentially in spiral fashion. This conjecture is known to be false, both for general cubic polyhedra and within the specific class of fullerenes. Here we report counterexamples to the spiral conjecture within the 19 classes of cubic polyhedra with positive curvature, i.e., with no face size larger than six. The classes are defined by triples {p ₃, p ₄, p ₅} where p ₃, p ₄ and p ₅ are the respective numbers of triangular, tetragonal and pentagonal faces. In this notation, fullerenes are the class {0, 0, 12}. For 11 classes, the reported examples have minimum vertex number, but for the remaining 8 classes the examples are not guaranteed to be minimal. For cubic graphs that also allow faces of size larger than 6, counterexamples are common and occur early; we conjecture that every infinite class of cubic polyhedra described by allowed and forbidden face sizes contains non-spiral elements.     

An improved local branching approach for train formation planning

The train formation plan (TFP) determines routing and frequency of trains, and assigns the demands to trains. In this paper, an improved local branching algorithm is proposed for the TFP model in Iranian railway. This solution strategy is exact in nature, although it is designed to improve the heuristic behavior of the mixed integer programming (MIP) solver at hand. In the local branching algorithm, additional constraints are built in the model for the binary variables, but in the improved local branching algorithm, the additional constraints are built in the model for integer variables. A state-of-the-art method is applied for parameter tuning using design of experiments approach. To evaluate the proposed solution method, we have simulated and solved twenty test problems. The results show the efficiency and effectiveness of the proposed approach. The proposed algorithm is implemented for Iranian Railway network as a case study.     

Solid-state NMR investigations of Si-29 and N-15 enriched silicon nitride

We compare ²⁹Si magic-angle spinning (MAS) nuclear magnetic resonance (NMR) spectra from the two modifications of silicon nitride, α-Si₃N₄ and β-Si₃N₄, with that of a fully (²⁹Si, ¹⁵N)-enriched sample ²⁹Si₃¹⁵N₄, as well as ¹⁵N NMR spectra of Si₃¹⁵N₄ (having ²⁹Si at natural abundance) and ²⁹Si₃¹⁵N₄. We show that the ¹⁵N NMR peak-widths from the latter are dominated by J(²⁹Si–¹⁵N) through-bond interactions, leading to significantly broader NMR signals compared to those of Si₃¹⁵N₄. By fitting calculated ²⁹Si NMR spectra to experimental ones, we obtained an estimated coupling constant J(²⁹Si–¹⁵N) of 20 Hz. We provide ²⁹Si spin-lattice (T₁) relaxation data for the ²⁹Si₃¹⁵N₄ sample and chemical shift anisotropy results for the ²⁹Si site of β-Si₃N₄. Various factors potentially contributing to the ²⁹Si and ¹⁵N NMR peak-widths of the various silicon nitride specimens are discussed. We also provide powder X-ray diffraction (XRD) and mass spectrometry data of the samples.     

Synthesis of homo-propargylic ethers: A domino ring opening/coupling reaction of oxiranes with terminal alkynes and aryl iodides

A domino ring opening/cross-coupling reaction of oxiranes with terminal alkynes and aryl iodides has been developed. This transformation serves as a protocol for the synthesis of homo-alkyne ether skeletons from the readily available starting materials. The success of the reaction has dependence on catalyst/ligand system of choice. The synthesis utility of the alkyne ether skeletons in formation of chromane skeleton has also been studied.     

State‐of‐the‐Art and Trends in Synthesis,Properties, and Application of Quantum Dots‐Based Nanomaterials

Quantum dots (QDs) with a nanoscale size range have attracted significant attention in various areas of nanotechnology due to their unique properties. Different strategies for the synthesis of QD nanoparticles are reported in which various factors, such as size, impurities, shape, and crystallinity, affect the QDs fundamental properties. Consequently, to obtain QDs with appropriate physical properties, it is required to select a synthesis method which allows enough control over the surface chemistry of QDs through fine‐tuning of the synthesis parameters. Moreover, QDs nanocrystals are recently used in multidisciplinary research integrated with biological interfaces. The state‐of‐the‐art methods for synthesizing QDs and bioconjugation strategies to provide insight into various applications of these nanomaterials are discussed herein.     

Dynamic bifurcations analysis of a micro rotating shaft considering non-classical theory and internal damping

In this study, the dynamic bifurcation of a viscoelastic micro rotating shaft is investigated. The non-classical theory (the modified couple stress theory) and the Kelvin Voigt model are used for modeling the viscoelastic micro shaft. The transverse equations of motion are derived using the variational approach. The reduced order model of the system is obtained by the Galerkin method. Using the Routh–Hurwitz criteria the stability regions of the system are extracted in which the effect of the length scale parameter is significant. Using the center manifold theory and the normal form method the double zero eigenvalue bifurcation is analyzed. The results show that the internal and external damping coefficients, the rotational speed and the material length scale parameter influence the critical speed, amplitude, and phase of a non-trivial solution, and radius of limit cycle (periodic solution). Also, it is seen that by increasing the dimensionless length scale parameter (material length scale per radius of the shaft) the radius of the limit cycle is decreased, whereas the critical rotational speed and the rate of the phase are increased. However, the radius of the limit cycle concerning the classical theory is higher than that of regarding the modified couple stress theory. Furthermore, with an increase of the external damping coefficient the radius of the limit cycle is linearly decreased; however, the critical speed of the system is increased. Additionally, by decreasing length scale parameter the results of the modified couple stress theory approach the classical theory ones.