Kinetics of formation of barium tungstate in equimolar powder mixture of BaCO<Subscript>3</Subscript> and WO<Subscript>3</Subscript>

The formation of Barium monotungstate (BaWO₄) particles in equimolar powder mixtures of BaCO₃ and WO₃ was examined under isothermal and non-isothermal conditions upon heating in air at 25–1200 °C, using thermogravimetry. Concurrence of the observed mass loss (due to the release of CO₂) to the occurrence of the formation reaction was evidenced. Accordingly, the extent of reaction (x) was determined as a function of time (t) or temperature (T). The x–t and x–T data thus obtained were processed using well established mathematical apparatus and methods, in order to characterize nature of reaction rate-determining step, and derive isothermal and non-isothermal kinetic parameters. Moreover, the reaction mixture quenched at various temperatures (600–1,000 °C) in the reaction course was analyzed by various spectroscopic and microscopic techniques, for material characterization. The results obtained indicated that the reaction rate may be controlled by unidirectional diffusion of WO₃ species across the product layer (BaWO₄), which was implied to form on the barium carbonate particles. The isothermally determined activation energy (118–125 kJ/mol) was found to be more credible than that (245 kJ/mol) determined non-isothermally.     

Extraction of biogenic amines using sorbent materials containing immobilized crown ethers

Three sorbent materials (A18C6-MS, DA18C6-MS and AB18C6-MS) based on the crown ether ligands, 1-aza-18-crown-6, 1,4,10,13-tetraoxa-7,16-diazacyclo octadecane and 4′-aminobenzo-18-crown-6, respectively, were prepared by the chemical immobilization of the ligand onto mesoporous silica support. The sorbents were characterized by FT-IR, scanning electron microscopy-energy dispersive X-ray microanalysis, elemental analysis and nitrogen adsorption-desorption test. The applicability of the sorbents for the extraction of biogenic amines by the batch sorption method was extensively studied and evaluated as a function of pH, biogenic amines concentration, contact time and reusability. Under the optimized conditions, all the sorbents exhibited highest selectivity toward spermidine (SPD) compared to other biogenic amines (tryptamine, putrescine, histamine and tyramine). Among the sorbents, AB18C6-MS offer the highest capacity and best selectivity towards SPD in the presence of other biogenic amines. The AB18C6-MS sorbent can be repeatedly used three times as there was no significant degradation in the extraction of the biogenic amines (%E > 85). The optimized procedure was successfully applied for the separation of SPD in food samples prior to the reversed-phase high performance liquid chromatography separation.     

Synthesis of quinine and quinidine using sulfur ylide-mediated asymmetric epoxidation as a key step

The epoxidation of meroquinene aldehyde with a chiral sulfur ylide as the key step in the synthesis of quinine and quinidine is described. The epoxidation reactions proceed under reagent control with high selectivity and good yield. The effect of sulfide and ylide substituents on the stereochemical outcome of the reaction is discussed.     

Influence of gamma radiation on the colour strength and fastness properties of fabric using turmeric (Curcuma longa L.) as natural dye

The effect of gamma radiation on the dyeing of cotton with extract of turmeric (Curcuma longa L.) powder has been investigated. Cotton fabric and turmeric powder were irradiated to absorbed doses of 1, 2, 3, 4 and 6 kGy using Co-60 gamma irradiator. Dyeing parameters such as temperature, pH and mordant concentration were optimized. Dyeing was performed using un-irradiated and irradiated cotton with the extracts of un-irradiated and irradiated turmeric powder in order to investigate the effect of radiation treatment on the colour strength of dyed fabric. The reported data of un-irradiated and irradiated fabrics dyed with un-irradiated and irradiated dyes were obtained using the spectraflash SF-650. The colourfastness to light, rubbing- and washing-fastness properties showed that gamma irradiation has improved the dyeing characteristics from fair to good.     

Cyclization vs. Elimination Reactions of 5‐Aryl‐5‐hydroxy 1,3‐Diones: One‐Pot Synthesis of 2‐Aryl‐2,3‐dihydro‐4H‐pyran‐4‐ones

2‐Aryl‐2,3‐dihydro‐4H‐pyran‐4‐ones were prepared in one step by cyclocondensation of 1,3‐diketone dianions with aldehydes. The use of HCl (10%) for the aqueous workup proved to be very important to avoid elimination reactions of the 5‐aryl‐5‐hydroxy 1,3‐diones formed as intermediates. The TiCl₄‐mediated cyclization of a 2‐aryl‐2,3‐dihydro‐4H‐pyran‐4‐one with 1,3‐silyloxybuta‐1,3‐diene resulted in cleavage of the pyranone moiety and formation of a highly functionalized benzene derivative.     

Synthesis and biological studies of complexes of 2- amino-<Emphasis Type=Italic>N</Emphasis>(2-aminobenzoyl) benzohydrazide with Co(II), Ni(II), and Cu(II)

The present work is concerned with the synthesis and coordination compounds of 2-amino-N(2-aminobezoyl) benzohydrazide (ABH). The ligand was synthesized by the reaction of methylanthranilate and hydrazine in 2:1 molar ratio. It can be viewed as a modified form of hydrazide. The ligand was characterized by ¹H-NMR, ¹³C-NMR, mass spectrometry, elemental analysis, and infrared studies. The ligand has got -NH₂ moeity, the site for chelation. The complexes of Co(II), Ni(II), and Cu(II) chlorides and bromides were prepared. These complexes were characterized by elemental analysis, infrared, conductance, and magnetic susceptibility studies. Infrared spectra studies confirmed the formation of complexes, while elemental studies suggested the complexation of [M(ABH)X₂] (where X = Cl⁻ or Br⁻) composition.     

Effect of Temperature on Cd2+ Sorption by Mixed Oxides of Iron and Silicon

The current study focuses on the synthesis and sorption properties of two mixed oxides of iron and silicon prepared by physical mixing (M₁) and sequential precipitation methods (M₂). Both the mixed oxides were synthesized from equimolar ratios of Fe(OH)₃ and SiO₂ and characterized for surface area, EDX, XRD and PZC. The surface area, micropore volume and average pore width of the oxide M₁ were higher as compared to the oxide M₂. However, potentiometric titrations revealed that mixed oxide synthesized by this method had a very high capacity towards Cd²⁺ ions as compared to the mixed oxide M₁. Sorption of Cd²⁺ ions at pH 5 on mixed oxide, M₂ was found to increase with temperature in the range 288 to 318 K. Langmuir equation was found applicable to the sorption data with R²>0.99. Entropy (ΔS^?), enthalpy (ΔH^?) and free energy changes (ΔG^?) were calculated which revealed the process to be endothermic and spontaneous in nature.     

SiCl4-Zn induced reductive coupling of carbonyl compounds: novel and efficient routes for one-pot syntheses of 1,2,3-triaryl-2-propen-1-ones and pinacolones at room temperature

An unprecedented one-pot reductive trimerization of aromatic aldehydes to 1,2,3-triaryl-2-propen-1-ones as well as tandem reductive coupling-rearrangements of aryl ketones to pinacolone analogues was efficiently achieved using tetrachlorosilane-zinc at room temperature.     

Efficient enantioselective synthesis of tetramic acids and lactams from threonine

Regioselective Dieckmann and aldol cyclisations using an N-acyloxazolidine derived from threonine give substituted tetramic acids and pyroglutamates in high yield and enantioselectivity. These are easily deprotected under mild conditions to give products, some of which exhibit antibacterial activity.