BF3·OEt2-catalyzed synthesis of 1-(tetrahydropyran-3-yl)-1,3-dihydroisobenzofuran and trans-fused hexahydropyrano[3,2-c]chromene derivatives

A novel intramolecular Prins cyclization of (E)-5-(2-(hydroxymethyl)phenyl)pent-4-en-1-ol with aldehydes has been achieved using 10 mol % BF₃·Et₂O to produce 1-(tetrahydropyran-3-yl)-1,3-dihydroisobenzofuran derivatives in good to excellent yields with high selectivity. Similar type of coupling with salicylaldehydes provides the trans-fused hexahydropyrano[3,2-c]chromene derivatives in excellent yields.     

Determination of Required HLB of Capryol 90

The required hydrophilic-lipophilic balance (HLB) of an oily substance indicates the HLB of the surfactants required to prepare a stable emulsion using the oil. This study utilizes empirical method to calculate required HLB (RHLB) of Capryol 90 using surfactant blends (Span 20, Tween 20, vitamin E TPGS, Pluronic F68, Span 60, and Tween 80). The methods used were assessment of degree of creaming after centrifugation and after shelf storage for 28 days at room temperature, turbidimetric method, accelerated stability study, and droplet size analysis. The droplet size was found to be in the range of 15 to 2 µm and v/v% separation after centrifugation was found to be 0–82%. The RHLB for Capryol 90 was found to be 15. The effect of various surfactant blends was investigated. Results revealed that a blend of tocopherol polyethylene glycol succinate (TPGS) and Pluronic F68 gave the most stable emulsion for Capryol 90.     

Industrial Applications of Dimeric Surfactants: A Review

Dimeric surfactants also known as gemini surfactants have received lots of attention for high performance formulations in the various scientific and commercial products. Due to the greater amount of hydrocarbon per molecule, the critical micelle concentrations (CMC) of dimeric are typically one order of magnitude lower than the corresponding monomeric surfactant. They are ten to hundred times more efficient at reducing the surface tension of water and the interfacial tension of the oil-water interface than conventional surfactants. Besides, the Krafft temperatures of gemini surfactants with hydrophilic spacers are generally very low giving these surfactants the capacity to be used in cold water. These surfactants display a range of interesting properties, including elevated surface activity, extremely low CMC and extraordinary rheology and self-assimilation aspect. As a consequence of these properties, they have many potential applications include detergents and cleaning agents, cosmetics, textile, and dyeing, dispersion stabilization and emulsion polymerization, genetics science, pharmaceutical, and biological applications.      

Experimental and Theoretical Studies on Synthesized Compounds as Corrosion Inhibitor for Mild Steel in Hydrochloric Acid Solution

Imidazole derivatives, namely, 1-((1-(piperazinomethyl)-1H-benzoimidazol-2-yl)methyl)-2-phenylhydrazine (PBIP), and 1-((1-(morpholinomethyl)-1H-benzoimidazol-2-yl)methyl)-2-phenylhydrazine (MBIP) were synthesized and investigated as inhibitors for mild steel corrosion in 15% HCl solution using weight loss, potentiodynamic polarization, and electrochemical impedance spectroscopy (EIS) techniques. It was found that the inhibition efficiency of both the inhibitors increases with increase in concentration of inhibitors and decreases with increase in temperature. The inhibitors, PBIP and MBIP, show corrosion inhibition efficiency of 92.6% and 91.4% at 300 ppm concentration, respectively, at 303 K. Polarization studies showed that both the studied inhibitors were of mixed type in nature. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were performed for surface study of uninhibited and inhibited mild steel samples. The semi-empirical AM1 method was employed for theoretical calculations.     

Fluorimetric estimation of U(VI) in the presence of a large excess of Th(IV)

A fluorescence based method has been developed for the determination of trace amounts of uranium in thorium matrix using a mixture of phosphoric acid (H₃PO₄) and sulfuric acid (H₂SO₄), as fluorescence enhancing reagent for uranyl (UO₂ ²⁺) ion fluorescence. Synthetic samples mimicking the composition of ThO₂ fuel were prepared and the concentration of U(VI) was estimated. Satisfactory results are obtained when uranium is present at a concentration of 10 ppm in solid thorium samples with good precision.     

Structural interaction leading to volumetric changes in aqueous solutions of nitrates of rubidium,cesium, strontium,yttrium, and gallium at different temperatures

Densities of the aqueous dilute solutions of rubidium, cesium, strontium, yttrium, and gallium nitrate were measured at different temperatures ranging from (293.15–343.15) K and atmospheric pressure. From these density values, the apparent molal volumes were calculated and fitted to Masson’s correlation and the temperature dependence was correlated by a second order polynomial. The apparent molal volumes at infinite dilution and experimental slopes have been interpreted in terms of ion–solvent and ion–ion interactions, respectively. The measurements include density as per ASTM D-4052, refractive index (nD²⁵) at sodium D line at 25 °C. Thermal isobaric expansibility was calculated and structure making and structure breaking behaviour of electrolytes were inferred from the sign of the second derivative of apparent molal volumes with respect to temperature at constant pressure. The experimental apparent molal volume was compared with the available literature value.     

Kinetics of Pu(IV) sorption by smectite-rich natural clay

Kinetics of sorption of Pu(IV) by smectite-rich clay has been studied at varying metal ion concentrations. Different concentrations were achieved using different isotopes of Pu, namely, ²³⁹Pu, ²³⁸Pu and ²³⁷Pu. ²³⁷Pu was produced by alpha induced reaction on ²³⁵U, followed by radiochemical separation of Pu from irradiated U₃O₈ target. The concentrations used are above and below the solubility of Pu(IV) under neutral pH conditions, thereby, indicating the mechanism of sorption reactions of Pu(IV) in typical laboratory experiments and field level observations. Kinetics of Pu(IV) at 10^?13 M concentration was found to be fast whereas at higher metal concentration the rate is governed by a slow step, indicating the role of formation of Pu(IV) polymeric species at the sorbent surface.     

Quality by design: A systematic and rapid liquid chromatography and mass spectrometry method for eprosartan mesylate and its related impurities using a superficially porous particle column

The present work describes the systematic development of a robust, precise, and rapid reversed‐phase liquid chromatography method for the simultaneous determination of eprosartan mesylate and its six impurities using quality‐by‐design principles. The method was developed in two phases, screening and optimization. During the screening phase, the most suitable stationary phase, organic modifier, and pH were identified. The optimization was performed for secondary influential parameters—column temperature, gradient time, and flow rate using eight experiments—to examine multifactorial effects of parameters on the critical resolution and generated design space representing the robust region. A verification experiment was performed within the working design space and the model was found to be accurate. This study also describes other operating features of the column packed with superficially porous particles that allow very fast separations at pressures available in most liquid chromatography instruments. Successful chromatographic separation was achieved in less than 7 min using a fused‐core C₁₈ (100 mm × 2.1 mm, 2.6 μm) column with linear gradient elution of 10 mM ammonium formate (pH 3.0) and acetonitrile as the mobile phase. The method was validated for specificity, linearity, accuracy, precision, and robustness in compliance with the International Conference on Harmonization Q2 (R1) guidelines. The impurities were identified by liquid chromatography with mass spectrometry.     

An unusual conformation of gabapentin (Gpn) in Pyr‐Gpn‐NH‐NH‐Pyr stabilized by weak interactions

The crystal structure of N‐[(1‐{2‐oxo‐2‐[2‐(pyrazin‐2‐ylcarbonyl)hydrazin‐1‐yl]ethyl}cyclohexyl)methyl]pyrazine‐2‐carboxamide monohydrate (Pyr‐Gpn‐NN‐NH‐Pyr·H₂O), C₁₉H₂₃N₇O₃·H₂O, reveals an unusual trans–gauche (tg⁻) conformation for the gabapentin (Gpn) residue around the C^γ—C^β (θ₁) and C^β—C^α (θ₂) bonds. The molecular conformation is stabilized by intramolecular N—H...N hydrogen bonds and weak C—H...O interactions. The packing of the molecules in the crystal lattice shows a network of strong N—H...O and O—H...O hydrogen bonds together with weak C—H...O and π–π inteactions.     

Bioinspired Synthesis of Well‐Ordered Layered Organic–Inorganic Nanohybrids: Mimicking the Natural Processing of Nacre by Mineralization of Block Copolymer Templates

The unique mechanical performance of nacre, the pearly internal layer of shells, is highly dependent on its complex morphology. Inspired by the structure of nacre, the fabrication of well‐ordered layered inorganic–organic nanohybrids is presented herein. This biomimetic approach includes the use of a block copolymer template, consisting of hydrophobic poly(vinylidene fluoride) (PVDF) lamellae covered with hydrophilic poly(methacrylic acid) (PMAA), to direct silica (SiO₂) mineralization. The resulting PVDF/PMAA/SiO₂ nanohybrid material resembles biogenic nacre with respect to its well‐ordered and layered nanostructure, alternating organic–inorganic phases, macromolecular template, and mild processing conditions.