The novel ?-phosphorus labile ylide of 1-(p-tolyl)-2-(tri-p-tolylphosphoranylidene)ethanone (PTTPPY) is prepared by the reaction of 2-bromo-1-(p-tolyl)ethanone with tri-p-tolylphosphine in chloroform as solvent. The complexes of the type [HgX2(p-tolyl)3PCHCOC6H4CH3)] (X = Cl, Br and I) are prepared by the reaction of title ylide with mercury(II) halides in good yields, using methanol as solvent. The final products were characterized by IR, 1H, 13C, 31P NMR spectroscopic methods and microanalysis.
Kinetics of the oxidation of primary aliphatic alcohols has been carried out using phase transferred monochromate in benzene. Tetrabutylammonium bromide (TBAB) and tetrabutylphosphonium bromide (TBPB) are used as phase transfer catalysts (PT catalyst). The reaction shows first order dependence on both [alcohol] and [monochromate ion]. The oxidation leads to the formation of corresponding aldehyde and no traces of carboxylic acid has been detected. The reaction mixture failed to induce the polymerization of added acrylonitrile which rules out the presence radical intermediates in the reaction. Various thermodynamic parameters have been evaluated and a suitable mechanism has been proposed.
In this work, acidity constants protonated form of 4.4 & apos; -bis astilbene-2,2 & apos; -disulfonic-disodium salts (TRIAZ) have been determined spectrophotometrically and spectrofluorimetrically at 25?C and ionic strength of 0.1M KNO3. A program based on MCR-ALS applied for determination of acidity constants. The results show that the peak values of dye are influenced by the presence of anionic, cationic, and nonionic surfactants. The effects of sodium dodecyl sulfate (SDS), Triton X-100 (TX-100) and cetyl trimethyl ammonium bromide (CTAB) as a surface-active agent on the acidic and basic forms, and the spectral properties of dye were studied. Also, we determined the critical micelle concentration (CMC) for these surfactants by spectrophotometric and spectrofluorimetric triazine dye probes. In addition, by using of evolving factor analysis (EFA) and multivariate curve resolution alternative least squares (MCR-ALS) methods, acidity constants were acquired.
In this work, a variety of highly substituted quinolines were readily synthesized via Friedlander annulation using Br?nsted acid silica-based sulfonic acid as a modified catalyst under solvent-free conditions at room temperature. This efficient procedure has the advantages of giving the target compounds in high yields, short reaction times, simple workup procedure, reusability of the catalyst, and environmentally benign conditions.
The title compound 3-amino-5-(4-chlorophenyl)pyridazine-4-carbonitrile was prepared by a one-pot three-component reaction of malononitrile with corresponding arylglyoxal in the presence of hydrazine hydrate at room temperature in water and ethanol. Its structure was also con?rmed by its IR, 1H, 13C-NMR, Mass spectral data and elemental analysis. The compound was crystallized in the monoclinic system, space group P21/c, a = 3.817(3) ?, b = 13.533(10) ?, c = 19.607(15) ?, B = 93.401(10)°, Z=4, R1 = 0.0906 and wR2 = 0.1422. The crystal structure of the compound also shows a weak intermolecular interaction between N1 atom of one molecule and N3 atom of the other molecule.
Glacial acetic acid as a protic acid was employed as a catalyst in a solvent free condition for facile preparation of di(indolyl)methanes (DIMs) via one-pot condensation of indole with aryl or heteroaryl aldehydes. Various aryl and heteroaryl aldehydes were efficiently converted to the corresponding di(indolyl)methanes (1a-p) in high yields. The described novel synthetic method proposes several advantages of safety, mild condition, short reaction times, high yields, simplicity and the inexpensively glacial acetic acid compared to other catalysts.
A highly sensitive, accurate and simple spectrophotometric method was established for determination of naproxen (NAP). The method involved ion-pair complex formation between naproxen and bromophenol blue (BPB). The colored product was measured at 432 nm. The reaction conditions were optimized. The absorbance was found to increase linearly with increase in concentration of NAP which was corroborated by correlation coefficient value. Beer’s law was obeyed in the concentration range of 1-110 µg mL-1 with molar absorptivity of 9.756×103 L mol-1 cm-1. The limits of detection (LOD) and quantitation (LOQ) for the proposed method are 0.292 and 0.973 µg mL-1, respectively. Recovery of the method was carried out by standard addition method. Recovery studies and statistical data proved the accuracy, reproducibility and the precision of the proposed method. The common excipients did not interfere in this analysis. Hence the method is useful for routine estimation of naproxen in pharmaceutical formulation and human serum samples.
An inexpensive straightforward approach to direct oxidative twofold C-H arylation of 1,4-naphthoquinone catalyzed by readily available Br?nsted acids was developed. Under the simple and easily achievable reaction conditions, electron-rich aromatics undergo Friedel-Crafts type functionalization to furnish 2-arylonaphthoquinones in good yields. The attempt to rationalize the scope and limitation of the approach based on desktop PC DFT calculation and reactivity indexes theory was taken up.
Ferrocene and their derivatives are well-known redox active materials and were extensively used by construction of modified electrodes for the design of electrochemical sensors and biosensors. Substituent derivatization of ferrocene offers the prospect of controlling ferrocene moiety properties such as solubility, stability, reversibility of oxidation wave (important for their role as an electron transfer mediator) and oxidation potential, which is critical in the electrochemical determination of biological compounds. A new series of rigid alkynylferrocene including of 2-ferrocenylethynyl fluoren (3a), 2-ferrocenylethynyl fluoren-9-one (3b), 4-ferrocenylethynyl aniline (3c) and 3-ferrocenylethynyl-1-trifluoromethyl benzene (3d) have been prepared in good yields by Sonogashira coupling reaction. All products were characterized by 1H and 13C NMR, FT-IR, and elemental analysis. The redox chemistry of these compounds has been investigated by cyclic voltammetry. The half-wave potential of the terminal ferrocenyl moieties increases progressively in the order of 3c & LT; 3a & LT; 3b & LT; 3d, which is consistent with the electron density on the ferrocenyl unit.
A mild and efficient procedure has been proposed for oxidation of benzylic alcohols to the corresponding carbonyl compounds using polymer-supported dichloroiodate (PSDI). The oxidations were carried out in acetonitrile solution, affording the corresponding aldehydes or ketones in high substrate conversion and short reaction time under mild aprotic conditions. Excellent selectivity was observed between primary benzyl alcohols and secondary ones as well as non-benzylic alcohols in the oxidation reactions. The catalyst can be easily prepared and regenerated.