Ultrasound-assisted synthesis of novel spiro[indoline-3,5′-pyrido[2,3-d]pyrimidine] derivatives using Fe3O4@Propylsilane@Histidine[HSO4−] as an effective magnetic nanocatalyst

A simple, economical, three-component, and one-pot synthesis of novels spiro[indoline-3,5′-pyrido[2,3-d]pyrimidine] derivatives by condensation of dimethyl acetylene dicarboxylate, isatin derivatives, and 6-amino-1,3-dimethyluracil in presence of Fe₃O₄@Propylsilane@Histidine[HSO₄⁻] as an impressive catalyst via reflux and ultrasound procedure is described. The results show that ultrasound method has several advantages such as milder condition, shorter reaction time, and higher reaction yield.     

Advances in the design of nanomaterial-based electrochemical affinity and enzymatic biosensors for metabolic biomarkers: A review

This review (with 340 refs) focuses on methods for specific and sensitive detection of metabolites for diagnostic purposes, with particular emphasis on electrochemical nanomaterial-based sensors. It also covers novel candidate metabolites as potential biomarkers for diseases such as neurodegenerative diseases, autism spectrum disorder and hepatitis. Following an introduction into the field of metabolic biomarkers, a first major section classifies electrochemical biosensors according to the bioreceptor type (enzymatic, immuno, apta and peptide based sensors). A next section covers applications of nanomaterials in electrochemical biosensing (with subsections on the classification of nanomaterials, electrochemical approaches for signal generation and amplification using nanomaterials, and on nanomaterials as tags). A next large sections treats candidate metabolic biomarkers for diagnosis of diseases (in the context with metabolomics), with subsections on biomarkers for neurodegenerative diseases, autism spectrum disorder and hepatitis. The Conclusion addresses current challenges and future perspectives.

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Graphical abstract This review focuses on the recent developments in electrochemical biosensors based on the use of nanomaterials for the detection of metabolic biomarkers. It covers the critical metabolites for some diseases such as neurodegenerative diseases, autism spectrum disorder and hepatitis.

     

Conformational effect of silica-supported poly(octadecyl acrylate) on molecular-shape selectivity of polycyclic aromatic hydrocarbons in RP-HPLC.

Poly(octadecyl acrylate) with a terminal reactive group was synthesized by radical telomerization in various solvents. The polymers were grafted onto porous silica for use in RP-HPLC, and the molecular recognition ability was investigated along with the selectivity for the structural isomers of polycyclic aromatic hydrocarbons. The mechanism of selectivity was also investigated with differential scanning calorimetry and NMR spectroscopic observations.     

Bottleneck Problems: An Information and Estimation-Theoretic View

Information bottleneck (IB) and privacy funnel (PF) are two closely related optimization problems which have found applications in machine learning, design of privacy algorithms, capacity problems (e.g., Mrs. Gerber’s Lemma), and strong data processing inequalities, among others. In this work, we first investigate the functional properties of IB and PF through a unified theoretical framework. We then connect them to three information-theoretic coding problems, namely hypothesis testing against independence, noisy source coding, and dependence dilution. Leveraging these connections, we prove a new cardinality bound on the auxiliary variable in IB, making its computation more tractable for discrete random variables. In the second part, we introduce a general family of optimization problems, termed “bottleneck problems”, by replacing mutual information in IB and PF with other notions of mutual information, namely f-information and Arimoto’s mutual information. We then argue that, unlike IB and PF, these problems lead to easily interpretable guarantees in a variety of inference tasks with statistical constraints on accuracy and privacy. While the underlying optimization problems are non-convex, we develop a technique to evaluate bottleneck problems in closed form by equivalently expressing them in terms of lower convex or upper concave envelope of certain functions. By applying this technique to a binary case, we derive closed form expressions for several bottleneck problems.     

Synthesis of novel tetra- and pentacyclic benzosultam scaffolds via domino Knoevenagel hetero-Diels–Alder reactions in water

An efficient catalyst-free and diastereoselective synthesis of novel dihydropyrano[2,3-d]pyrimidine and dihydropyrano[3,2-c]chromen-annulated benzosultams is described. A number of (E)-N-(2-formylphenyl)-N-methyl-2-phenylethenesulfonamides were synthesized and underwent a one-pot domino Knoevenagel hetero-Diels–Alder reaction, respectively, with N,N-dimethylbarbituric acid and 4-hydroxycoumarin in water, giving the desired products, in moderate to excellent yields.     

Polymeric alkenoxy amino acid surfactants: I. Highly selective class of molecular micelles for chiral separation of beta-blockers

Two amino acid-based alkenoxy micelle polymers were synthesized for this study. These include polysodium N-undecenoxy carbonyl-L-leucinate (poly-L-SUCL) and polysodium N-undecenoxy carbonyl-L-isoleucinate (poly-L-SUCIL). The polymerization time and concentration of the synthesized micelle polymers were optimized by (1)H-nuclear magnetic resonance (NMR) and capillary electrophoresis (CE) experiments. Detailed physicochemical properties ((1)H NMR, critical micelle concentration (CMC), optical rotation, partial specific volume, aggregation number, and polarity) were determined, and these molecular micelles were introduced as a pseudostationary phase in micellar electrokinetic chromatography to study the molecular recognition and to develop a method for simultaneous separation of eight chiral beta-blockers. It is found that poly-L-SUCL gives overall better chiral resolution and wider chiral window than poly-L-SUCIL. After optimizing the type of micelle polymer, injection size and temperature, simultaneous separation and enantioseparation of eight beta-blockers were achieved in less than 35 min. A comparison with the amide-type surfactants of the same polar head group and alkyl chain length showed that carbamate-type surfactants always work better than the corresponding amide-type surfactant.     

Glycine-based polymeric surfactants with varied polar head group: II. chemical selectivity in micellar electrokinetic chromatography using linear solvation energy relationships

A series of four acyl and four alkenoxy glycinates (i.e., mono-, di-, tri-, and tetraderivatives of polysodium N-undecenoyl glycinate (poly-SUGs) as well as polysodium N-undecenoxy carbonyl glycinates (poly-SUCGs)) were compared for simultaneous separation of nonhydrogen bonding (NHB), hydrogen-bond acceptor (HBA), and hydrogen-bond donor (HBD) solutes. An increase in the number of glycine units in the polar head group of polymeric surfactant decreases both the retention and the migration window of all solutes with some changes in separation selectivity. The poly(sodium N-undecenoxy carbonyl-glycinate) (poly-SUCG1) with one glycine unit was the least polar surfactant and has the lowest phase ratio, but this monoglycinate surfactant provided the best simultaneous separation of 10-NHBs and 8-HBAs. On the other hand, 9-HBDs were well separated using any of the six mono-, di-, and triglycinate surfactants compared to the two tetraglycinates. Linear solvation energy relationships (LSERs) and separation of the geometrical isomers studies were also performed to further envisage the selectivity differences. From LSER studies, the phase ratio and hydrogen-bond-donating strength of the poly-SUG series of surfactant were found to increase with an increase in the size of the head group, but no clear trends were observed for poly-SUCG surfactants. The cohesiveness for all poly-SUG and poly-SUCG was positive, but the values were generally lower (with exception of the poly(sodium N-undecenoyl glycyl-glycyl-glycinate)) at a higher number of glycine units. Finally, the poly(sodium N-undecenoyl glycinate) and poly-SUCG1 were found to be the two best polymeric surfactants as they provided relatively higher shape selectivity for separation of two of the three sets of geometrical isomers.     

Synthesis, structure, and magnetic properties of the layered copper(II) oxide Na2Cu2TeO6

A new quaternary layered transition-metal oxide, Na2Cu2TeO6, has been synthesized under air using stoichiometric (with respect to the cationic elements) mixtures of Na2CO3, CuO, and TeO2. Na2Cu2TeO6 crystallizes in the monoclinic space group C2/m with a = 5.7059(6) A, b = 8.6751(9) A, c = 5.9380(6) A, beta = 113.740(2) degrees, V = 269.05(5) A3, and Z = 2, as determined by single-crystal X-ray diffraction. The structure is composed of infinity(2)[Cu2TeO6] layers with the Na atoms located in the octahedral voids between the layers. Na2Cu2TeO6 is a green nonmetallic compound, in agreement with the electronic structure calculation and electrical resistance measurement. The magnetic susceptibility shows Curie-Weiss behavior between 300 and 600 K with an effective moment of 1.85(2) muB/Cu(II) and theta(c) = -87(6) K. A broad maximum at 160 K is interpreted as arising from short-range one-dimensional antiferromagnetic correlations. With the aid of the technique of magnetic dimers, the short-range order was analyzed in terms of an alternating chain model, with the surprising result that the stronger intrachain coupling involves a super-superexchange pathway with a Cu-Cu separation of >5 A. The J2/J1 ratio within the alternating chain refined to 0.10(1), and the spin gap is estimated to be 127 K.     

A vertical heat pipe: an experimental and statistical study of the thermal performance in the presence of low-frequency vibrations

New experimental results present the effects of low-frequency vibrations in a vertical heat pipe. The thermal resistance was investigated under different heat transfer rates, filling ratios and frequencies, increase of which improved the thermal performance. The vibrations were effective 33.83 % on the performance, and the best performance was estimated using the L16 array of Taguchi method, and it was achieved with the thermal resistance 0.064 K/W in the frequency 30 Hz.