One-pot and two-pot methods for chalcone derived pyrimidines synthesis and applications

Chalcone-derived pyrimidine is a well-known heterocyclic compound that is commonly present in ribonucleic acid (RNA) and deoxyribonucleic acid (DNA) bio-isosteres. Pyrimidine derivatives are effective in both the electronic industry and drug industries. This review highlights the synthesis of pyrimidines, namely mono-pyrimidine, bis-pyrimidine, fused pyrimidine, symmetric, and asymmetric pyrimidine via one-pot and two-pot methods. The one-pot method is the direct reaction of amino derivatives with aldehydes and acetophenones, whereas the two-pot method is frequently reported for the synthesis of chalcone before the cyclization to a pyrimidine. This review is important in organic synthesis, particularly in the heterocyclic field, regarding pyrimidines and their significance in therapeutic and electronic industries.     

Enhancing signal to noise ratio by fine-tuning tapers of cladded/uncladded buffer rods in ultrasonic time domain reflectometry in smelters

Buffer rods (BR) as waveguides in ultrasonic time domain reflectometry (TDR) can somewhat extend the range of industrial applications of ultrasonics. Level, temperature and flow measurements involving elevated temperatures, corrosive fluids and generally harsh environments are some of the applications in which conventional ultrasonic transducers cannot be used directly in contact with the media. In such cases, BRs with some design modifications can make ultrasonic TDR measurements possible with limited success. This paper deals with TDR in conjunction with distance measurements in extremely hot fluids, using conventional ultrasonic transducers in combination with BRs. When using BRs in the ultrasonic measurement systems in extreme temperatures, problems associated with size and the material of the buffer, have to be addressed. The resonant frequency of the transducer and the relative size of the transducer with respect to the diameter of BR are also important parameters influencing the signal to noise ratio (SNR) of the signal processing system used in the ultrasonic TDR. This paper gives an overview of design aspects related to the BRs with special emphasis on tapers and cladding used on BRs. As protective cladding, zirconium oxide–yttrium oxide composite was used, with its proven thermal stability in withstanding temperatures in rocket and jet engines up to 1650 °C. In general a BR should guide the signals through to the medium and from and back to the transducer without excessive attenuation and at the same time not exacerbate the noise in the measurement system. The SNR is the decisive performance indicator to consider in the design of BR based ultrasonic TDR, along with appropriate transducer, with suitable size and operating frequency. This work presents and analyses results from extensive experiments related to fine-tuning both geometry of and signals in cladded/uncladded BRs used in high temperature ultrasonic TDR with focus on overall performance based on measured values of SNR.     

Composition dependence of polymorphism and electrical conductivity in Ce(IV)-doped Bi4V2O11

For the first time, a new member of the BIMEVOX family, namely BICEVOX, has been synthesized by the partial solid-state substitution of Ce(IV) for vanadium in parent Bi₄V₂O₁₁ solid electrolyte. The electrical conductivity in Bi₄Ce _x V_{2? x} O_{11?( x /2)? δ} has been investigated in the compositional range 0 ≤ x ≤ 0.30, using FT-IR, X-ray powder diffraction, differential thermal analysis and ac impedance spectroscopy. Owing to the long-term stabilization of α- and β-polymorphs compared to other members of the BIMEVOX family, the BICEVOX system may be a prospective solid electrolyte for intermediate temperature solid oxide fuel cells due to the significantly increased conductivity at lower temperatures observed for the compositions x > 0.20.     

Effect of Ni(II) substitution on phase stabilization electrical properties of BICo(III)VOX.20 oxide-ion conductor

The BICO_0.20–xNI_xVOX solid electrolyte was synthesized by the standard solid-state reaction. The effect of Ni(II) substitution for Co(III) on phase stabilization and oxide-ion performance has been investigated in the compositional range 0?≤?x?≤?0.20 using X-ray powder diffraction, differential thermal analysis and AC impedance spectroscopy. The highly conductive γ′-phase was effectively stabilized at room temperature for compositions with x?≥?0.13 whose thermal stability increases with Ni content. The complex plane plots of impedance were typically represented at temperatures below 380?°C, suggesting a major contribution of polycrystalline grains to the overall electrical conductivity. The dielectric permittivity measurements revealed the fact that suppression of the ferroelectric transition is compositionally dependent. Interestingly, the maximum ionic conductivity at lower temperatures (~2.56?×?10^?4?S^?cm^?1 at 300?°C) was observed for the composition with x?=?0.13. The variation of low-temperature conductivity with Ni content was accompanied with a general drop in the corresponding values of ΔE_LT. However, the local minimum high-temperature conductivity, σ₆₀₀?°C?~?2.26?×?10^?2?S^?cm^?1 for x?=?0.10, coupled with a local maximum value of ΔE_HT?~?0.48?eV was attributed to an increased defect trapping effect correlated with the V(V)?→?V(IV) reduction at elevated temperatures.     

Edge-clique graphs

The edge-clique graphK(G) of a graphG is that graph whose vertices correspond to the edges ofG and where two vertices ofK(G) are adjacent whenever the corresponding edges ofG belong to a common clique. It is shown that every edge-clique graph is a clique graph, and that ifG is either an interval graph or a line graph, then so too isK(G). An algorithm is provided for determining whether a graph is an edge-clique graph. A new graph called the STP graph is introduced and a relationship involving this graph, the edge-clique graph, and the line graph is presented. The STP graphs are also characterized.Research supported in part by Office of Naval Research Contract N00014-88-K-0018.Research supported in part by Office of Naval Research Contract N00014-88-K-0163.     

Solid-state 13C NMR study of poly(vinyl alcohol) gels

Poly(vinyl alcohol) (PVA) with 55% and 61% syndiotacticity, and their related dry and hydrated gels obtained by two different freeze–thawing cycles have been investigated using the solid-state ¹³C CP-MAS NMR technique. From a comparative analysis of the spectra, evidence was obtained that the gelation process largely disrupts the intramolecular hydrogen-bonded network of the PVA. The addition of water to the dry gels favours their swelling, destroying intra-chain hydrogen bonds between hydroxyl groups as a function of the degree of tacticity and the gelation procedure, and promotes the formation of new networks of interchain hydrogen bonds. Information on the dynamics of the polymeric domains in the kilohertz range has been obtained from the analysis of the spin relaxation times T_1ρ(¹H) and T_1ρ(¹³C), indicating that homogeneous arrangements of the amorphous or swollen polymeric chains exist, independent of the preparation method or the tacticity of the PVA chains.     

Ion chemistry of α-diazoketones. 2. Synthesis of Ionized or protonated N-tosylpyrrolidin-3-ones from 1-diazo-4-tosylaminobutan-2-ones under electron impact or chemical ionization

Mass spectral syntheses of gaseous ionized or protonated N-tosylpyrrolidin-3-ones from 1-diazo-4-tosylaminobutan-2-one substrates under electron impact or protonating chemical ionization conditions, respectively, are supported by collisional activation experiments.     

Application of the StrOligo algorithm for the automated structure assignment of complex N-linked glycans from glycoproteins using tandem mass spectrometry

Oligosaccharides associated with proteins are known to give these molecules specific conformations and functions. Analysis of proteins would not be complete without studying the glycans. However, high-throughput techniques in proteomics will soon overwhelm the current capacity of methods if no automation is incorporated into glycomics. New capabilities of the StrOligo algorithm introduced for this purpose (Ethier et al., Rapid Commun. Mass Spectrom., 2002; 16: 1743) will be discussed here. Experimental tandem mass spectra were acquired to test the algorithm using a hybrid quadrupole-time-of-flight (QqTOF) instrument with a matrix-assisted laser desorption/ionization (MALDI) source. The samples were N-linked oligosaccharides from monoclonal antibody IgG, beta interferon and fetuin, detached by enzymatic deglycosylation and labeled at the reducing end. Improvements to the program were made in order to reduce the need for user intervention. StrOligo strips the spectra down to monoisotopic peaks only. The algorithm first builds a relationship tree, accounting for each observed loss of a monosaccharide moiety, and then analyzes the tree and proposes possible structures from combinations of adducts and fragment ion types. A score, which reflects agreement with experimental results, is then given to each proposed structure. The program then decides which combination is the best one and labels relevant peaks in the experimental mass spectrum using a modified nomenclature. The usefulness of the algorithm has been demonstrated by assigning structures to several glycans released from glycoproteins. The analysis was completed in less than 2 minutes for any glycan, which is a substantial improvement over manual interpretation.     

An 27Al NMR study of complexes between Al3+ and imidazolidine-2-one in concentrated aqueous solution

The complexation between Al³⁺ and imidazolidine-2-one was investigated by ²⁷Al NMR spectroscopy at variable temperature. Several complexes with different stoichiometries were indentified. A fitting procedure based on the exchange modified Bloch equations and the Gauss-Newton method furnished the populations and exchange rates. From these the pertinent thermodynamic parameters were found.