Synthesis and Chemistry of 4-Aroyl-3-oxo- and 3-Chloropyridazine Derivatives

4H,5H-6-Phenyl (1a) and 6-p-phenoxyphenyl (1b) pyridazin-3(2H)-ones were reacted with aromatic aldehydes to give 4-arylmethylpyridazm-3(2H)-ones (2a-g), Oxidation of (2a-g) with various oxidising agents (selenium dioxide in ethanol or chromium trioxide in acetic acid) gave 4-aroyl-6-arylpyridazin-3(2H)-ones (3a-g). Chlorination of (3a-g) with phosphorous oxychloride afforded 4-aroyl-6-aryl-3-chloropyridazine (4a-g). 1H-3-Aryl-5-phenylpyrazolo[3,4-c]pyridazines (5a-d) were obtained by heating (4a-d) with excess hydrazine hydrate. Hydroxyamination of (3e-g) with iydroxylamine gave aryl-4(6-p-phenoxyphenyl-2,3-dihydro-3-oxo)pyridazinyl oxime (6a-c). Silylation of oximes (6b & 6c) gave (7a & 7b) as acyclic compound instead of the expected seven - membered - ring compound (8).     

Synthesis and Crystal Structure of [Pb(trz)(tfpb)(H2O)]: a Lead(II) Complex Containing 2,4,6‐Tris(2‐pyridyl)‐1,3,5‐triazine and 4,4,4‐Trifluoro‐1‐phenyl‐1,3‐butandionate

[Pb(trz)(tfpb)(H₂O)] ( 1 ) (trz and tfpb are the abbreviations of 2,4,6‐tris(2‐pyridyl)‐1,3,5‐triazine and 4,4,4‐trifluoro‐1‐phenyl‐1,3‐butandionate, respectively) have been synthesized and characterized by elemental analysis and IR, ¹H NMR, spectroscopy. The single‐crystal structure of 1 shows the coordination number of the Pb²⁺ ions is eight with three N‐donor atoms from a “trz” ligand and four O‐donors from the dionate ligand and one molecule of water. The supramolecular features in this complex are guided by lone pair activity and control of strong hydrogen bonds, weak directional intermolecular interactions and aromatic π‐π stacking interactions.     

Zum Mechanismus der Ninhydrin-Reduktion nach polarographischen Untersuchungen in methanolischen Lösungen

Zusammenfassung Ergebnisse der polarographischen Reduktion von Ninhydrin in wasserfr. methanol. Lösungen werden mitgeteilt. Der Einfluß von Protonendonatoren (z. B. Benzoesäure) sowie von Substanzen, welche Protonisierungsreaktionen und die Wasserstoffabscheidung katalysieren (z. B. N,N-Dimethyl-p-phenylendiamin=DMPD) wird ermittelt. Unter bestimmten Bedingungen wird auch die dritte, soloatisierte Ketogruppe reduzierbar. Die Desoloatation wird auf die stufenweise Abdissoziation von H⁺ und OH^– bzw. OR^– zurückgeführt.Das an der Elektrodenoberfläche adsorbierteDMPD wirkt bei der Reduktion der freien Ketogruppen als Protonenüberträger, bei der Reduktion der soloatisierten aber auch als Protonenakzeptor.Die exper. Ergebnisse der polarographischen Reduktion in methanol. Lösung stützen den aus vorangegangenen Untersuchungen in wäßr. Lösung aufgestellten Reduktionsmechanismus.

---

The polarographic behaviour of ninhydrin is investigated in water-free methanolic solutions. The effect of addition of protondonors (e.g., benzoic acid) and of substances catalyzing protontransfer-and hydrogen-discharge-reactions (e.g., N,N-dimethyl-p-phenylenediamine=DMPD) on the characteristics of the polarographic waves is described. Under well defined conditions all three keto-groups can be reduced. The reduction of the soloated keto-group involves the elimination of water by stepwise dissociation of H⁺ and OH^– (OR^–) ions. DMPD, adsorbed on the surface of the electrode, acts as proton-carrier in the reduction of the two free keto-groups, and also as proton-acceptor in the reduction of the third, soloated group.The experimental results of the polarographic reduction of ninhydrin in methanol confirm the mechanism of reduction in aqueous solutions previously presented.

---

---

Mit 2 Abbildungen     

Fabrication of optically transparent chitin nanocomposites

This paper demonstrates the preparation of chitin nanofibers from crab shells using a simple mechanical treatment. The nanofibers are small enough to retain the transparency of neat acrylic resin. Possessing hydroxyl and amine/N-acetyl functionalities, water suspension of chitin nanofibers was vacuum-filtered 9 times faster than cellulose nanofibers to prepare a nanofiber sheet of 90 mm in diameter. This is a prominent advantage of chitin nanofibers over cellulose nanofibers in terms of commercial application. Interestingly, chitin acrylic resin films exhibited much higher transparency than cellulose acrylic resin films owing to the close affinity between less hydrophilic chitin and hydrophobic resin. Furthermore, the incorporation of chitin nanofibers contributes to the significant improvement of the thermal expansion and mechanical properties of the neat acrylic resin. The properties of high light transmittance and low thermal expansion make chitin nanocomposites promising candidates for the substrate in a continuous roll-to-roll process in the manufacturing of various optoelectronic devices such as flat panel displays, bendable displays, and solar cells.     

Ion population fraction calculations using improved screened hydrogenic model with l-splitting

Ion population fraction(IPF) calculations are very important to understand the radiative spectrum emitted from the hot dense matter. IPF calculations require detailed knowledge of all the ions and correlation interactions between the electrons of an ion which are present in a plasma environment. The average atom models, e.g., screened hydrogenic model with l-splitting(SHML), now have the capabilities for such calculations and are becoming more popular for in line plasma calculations. In our previous work [Ali A, Shabbir Naz G, Shahzad M S, Kouser R, Rehman A and Nasim M H 2018 High Energy Density Phys. 26 48], we have improved the continuum lowering model and included the exchange and correlation effects in SHML. This study presents the calculation of IPF using classical theory of fluctuation for our improved screened hydrogenic model with l-splitting(I-SHML) under local thermodynamic equilibrium conditions for iron and aluminum plasma over a wide range of densities and temperatures. We have compared our results with other models and have found a very good agreement among them.     

Dechlorination of 2,4-dichlorophenoxyacetic acid using biochar-supported nano-palladium/iron: Preparation,characterization, and influencing factors

In the present study, peanut shell, a green waste raw material, was used to prepare biochar (BC) and to obtain BC-supported nano-palladium/iron (BC-nPd/Fe) composites for removing 2,4-dichlorophenoxyacetic acid (2,4-D) from water. Characterization analysis demonstrated that nPd/Fe particles were well dispersed on the BC surface with weakened magnetic properties. The average particle diameter and specific surface area of nPd/Fe were 101.3 nm and 6.7 m² g⁻¹, whereas the corresponding values of the BC-nPd/Fe materials were 88.8 nm and 14.8 m² g⁻¹, respectively. Several factors were found to influence the dechlorination of 2,4-D, including the weight ratio of BC to Fe, Pd loading ratio, initial solution pH, 2,4-D concentration, and reaction temperature. Dechlorination results indicated that the 2,4-D removal and phenoxyacetic acid (PA) generation rates were 44.1% and 20.1%, respectively, in the nPd/Fe system, and 100.0% and 92.1%, respectively, in the BC-nPd/Fe system. The dechlorination of 2,4-D was well described by the pseudo-first-order kinetic model (R² > 0.97), and the observed rate constants k_obs were 0.0042 min (nPd/Fe) and 0.0578 min (BC-nPd/Fe), respectively. The reaction mechanism indicated that the dechlorination hydrogenation was the main process to remove 2,4-D from water in the BC-nPd/Fe system. In addition, BC inhibited the formation of a passivation layer on the particle surface during the reaction, thus maintaining the high reactivity of BC-nPd/Fe. The easy preparation technique, high 2,4-D dechlorination capacity, and mild reaction conditions suggest that BC-nPd/Fe may be a promising alternative composite to remove 2,4-D from water.     

Measuring thickness of translucent plastic by scanner

Thickness measurement is important in various engineering fields. The several methods have been used to measure the thickness. This work explains a novel method for measuring the thickness of translucent plastic materials using scanner. The plastic samples were scanned against a white and a black background and the RGB parameters of obtained images were used to measure the opacity. Then, the thickness was calculated using relationship between thickness and opacity of samples. The best thickness prediction was obtained using a 3rd polynomial regression with the XYZ parameter.     

Preparation and validation of [67Ga]Ga-phytate kit and Monte Carlo dosimetry: an effort toward developing an impressive lymphoscintigraphy tracer

Journal of Radioanalytical and Nuclear Chemistry - Radiocolloides are essential for the detection of metastatic lymph nodes in breast cancer. In this study [67Ga]Ga-phytate, as an long-lived...     

Exploring and modeling the ion mobility spectrometry of perindopril: Example of protonation-dissociation reactions in large molecules

The current research is constructed for considering the chemical ionization and dissociation of perindopril in the positive mode of corona discharge ion mobility spectrometry. Four product ion peaks are observed in the ion mobility spectrum of perindopril erbumine at the cell temperature of 473 K. These peaks are assigned through the obtained intensity variation analysis in the ion mobility spectra over the elapsed time accompanied by the calculations backed by the validated density functional theory (DFT). In this regard, the most stable ionic species associated with each peak and the corresponding reliable generation pathways are found by the well-confirmed meta hybrid density functional method, M06-2X. The peaks are assigned to the protonated perindopril and its dissociation products, including counter ion and the related fragment ions. However, the structures of the neutral perindopril in the gas phase are thoroughly assessed to find a more stable one. The predicted chemical ionization products by the theory are in excellent agreement with our presented experiment here. Theoretical evaluations demonstrated that the production of a fragment by dissociation process occurs when perindopril gets a proton from the ionization region. Also, without protons, there is no dissociation process. Therefore, our mechanism investigated here is the proton transfer one. All possible sites of perindopril are considered theoretically for protonation along with their possible reactions. In addition to the computed PES, the assigned ions for obtained spectra are confirmed by the computed equilibrium constants and rate constants. Our theoretical results show that the peak of the main fragment is for M-CH₃CH₂OH produced by a reaction pathway involving no barrier. This study opens new perspectives in interpreting large molecules spectra for future studies.