Vol. 2 & Issue 4 ; Section A : Chemical Sciences

Date : Aug. to Oct.2012

 

Potentiometric Study of Menadione Complexes with Transition Metals in DMSO- Water and DMF-Water Medium

Milind N. Gaikwad, Suresh T. Gaikwad, Anjali S. Rajbhoj

  • Abstract

    Vitamin K complexes with transition metals in 37.5% (v/v) DMSO- water and 28%(v/v) DMF- water medium The stability constants for the transition metals with menadione have been studied using pH-measurements in 37.5% (v/v) DMSO- water and 28%.(v/v) DMF- water medium. The values of proton- ligand stability constant and metal- ligand stability constants were calculated. The overall stability constants were determined and are quoted

Synthesis, Structural Elucidation and Antimicrobial Activities of Some Novel Macrocyclic Complexes of Ni (II) Having thiaaza Potential Donors in 18-24 Membered Rings

Vivek G. Dave and Piyush J. Vyas

  • Abstract

    Macrocyclic complexes of Ni(II) having N2S2 potential donors in 18-24 membered rings, of the general formula: Ni(L1-5)X2, Where X=Cl-,CH3COO-,NO3- and L(1-5) is Macrocyclic ligands have been synthesized from the reaction of Nickel(II) salt, Dicarboxylic acids and p-aminothiophenol in 1:2:2 moler ratio in methanol. These complexes have been characterized by elemental analysis, molar conductance, molecular weight determination, IR spectra, reflectance spectra, thermo gravimetric analysis and magnetic measurements. Molecular weight determination of these complexes indicates their monomeric nature. Octahedral structure has been proposed on the basis of Spectrul data, magnetic data, Reflectance spectra, and Magnetic measurements. Two sulphur atoms and two nitrogen atoms of the macrocyclic ring coordinate to the central nickel ion in the square planar form in unidentate behavior. Antimicrobial activities of these complexes have been studied by screening them against fungi, such as Aspergillus flavus, Fusarium oxysporum, Trichoderma harzianum, and bacteria, such as Salmonella typhi and Bacillus subtili. Thise macrocyclic complexes were found to be more fungitoxic and antibacterial than bavestin and streptomycin taking as a standered.

Montmorillonite K-10 Catalysed Synthesis of 1-Aryl-3- Alkyl Substituted Indazoles

Hangirgekar S.P

  • Abstract

    A clean and simple method for the preparation of substituted indazoles was developed using the montmorillonite K-10 catalyzed reaction of 2-hydroxy acetophenone and hydrazine in methanol solvent. Good functional group compatibility was observed under mild reaction conditions and various substituted indazoles were obtained in moderate to excellent yield.

A Facile Route to the Synthesis of 8-[2’-(3”, 5”- Dimethyl-4”-Ethoxy Carbonyl Pyrrolyl) Hydrazine] Substituted Phenothiazines and their Biological Activity

M. N. Narule

  • Abstract

    A short facile synthesis of 8-[2’-(3’’, 5’’-dimethyl-4’’-ethoxy carbonyl pyrrolyl) hydrazine] substituted phenothiazines (5a-j) from 2-arylamin benzal-2-(3′,5′-dimethyl-4′-ethoxy carbonyl pyrrole)hydrazines(4) in presence of sulphur and iodine.These compounds were screened for their antibacterial activity against S. aureus and E. coli as well as for their antifungal activity against C. albicans and A. niger. The synthesized compounds are characterized by FTIR, 1H NMR, elemental and chemical properties

Quantitative Analysis of Quercetin in Pueraria Tuberosa by Using High Performance Liquid Chromatography

Bharti Jain and Rashmi Raghuvanshi

  • Abstract

    A simple, reproducible and efficient reverse phase high performance liquid chromatographic method has been developed and described for the quantitative determination of quercetin the root tuber powder of Pueraria tuberosa. The analysis was done at room temperature with a Promosil C18 column (250mm´4.60mm i.d.,5μm particle size) as stationery phase at a wavelength of 267nm for detection and determination. The mobile phase consisted of water: acetonitrile : acetic acid (90:10:0.2 v/v/v) at a flow rate of 1ml/min.The quercetin content of 66.7% was found in the ethanolic extract of crude Pueraria tuberosa. The proposed method is precise, sensitive, reproducible and easy to perform which can be effectively used for detection, monitoring and quantification of the flavonoid quercetin in Pueraria tuberosa.

Synthesis and Fluorescence study of Novel4-{4-[(2 Z)-2- (2-hydroxybenzyli dene) hydrazine] benzyl}- 1, 3 oxazolid in-2-one

B. R. Thorat, Sudhir Sawant, Mustapha Mandewale, Ramesh S. Yamgar and Ramdas G. Atram

  • Abstract

    The pharmaceutical important 4-(4-hydrazinylbenzyl)-1,3-oxazolidin-2-one hydrochloride (1) is condensed with salicylaldehyde (2) in methanol in presence of sodium methoxide forming schiff base 4-{4-[(2Z)-2-(2-hydroxybenzylidene)hydrazinyl]benzyl}-1,3-oxazolidin-2-one (3). It is characterized by TLC, FT-IR, and NMR spectroscopy. The IR peak at 1781, 3318 and 3230 cm-1 is due to O-CO-NH, -CO-NH- and =N-NH- stretching vibrations. The new peak at 1616 cm-1 is due to – C=N- (imino) group. The compound (3) is further subjected to fluorescence study. The Schiff base (3) shows excitation at 276 nm (ε 9.203) and 400 nm (ε 3.129) and émission at 413 nm (ε 580) for excitation at 276 nm & 403 nm (ε 234.58) and 403 nm (ε 432.70) for the excitation at 400 nm.

Estimation of Thiosalicylic Acid Using Photochemical Exchange Reaction of Sodium Nitroprusside

Gautam Kishor Sharma, Gayatri Prasad, T.R. Thapak, Arpan Bhardwaj and D.S. Raghuwanshi

  • Abstract

    A novel, rapid, faster and reliable quantitative method has been established for the determination of thiosalicylic acid using sodium nitroprusside as a spectroscopic probe. This method indicates that the sodium nitroprusside can react with the salicylic acid to form a colored product in the light reaction. Sodium nitroprusside is a photolabile complex and it undergoes photochemical ligand exchange reactions rapidly. The absorbance of the product is measured at the maximal absorption wavelength of 395.5 nm, and the amount of thiosalicylic acid can be calculated based on this absorbance by using calibration curve. The good linear relationship of the concentration of thiosalicylic acid versus absorbance is observed with a linear range of 1.48 x 10-4 – 9.50 x 10-4. The linear regression equation is A = 0.012x + 0.188, with the correlation coefficient of 0.998. The effects of different parameters like pH, change of concentration of sodium nitroprusside, concentration of ligands, light intensity etc. on percentage error were investigated. The efforts were made to minimize the percentage error and some optimum conditions were obtained. The progress of photochemical reaction for sample solution has been observed spectro-photochemically and the product was isolated and characterized. A tentative mechanism for this reaction has been proposed.

     

Preparation, Characterization, Antibacterial and DNA Binding Studies of Phenylenediamine Mixed Ligand Complex of Copper (II) Benzoate

Ramasubbu Rajakumar, Natarajan Raman and Sankaran Rajeswari

  • Abstract

    A new phenylenediamine mixed ligand complex of copper (II) benzoate was prepared. It was characterized by conductivity, magnetic susceptibility measurement, UV-Vis and IR spectral studies. Conductivity study concludes that the complex is a non-electrolyte. The remaining studies conclude the octahedral geometry around copper ion. The antibacterial activity of the title compound was compared with parent ligand and complex. DNA binding study was carried out with HS-DNA by absorption spectral technique. The binding constant was found to be 1.7 × 104.

Synthesis and Characterization of Some New Oxygen Containing Heterocyclic Compounds

Disha Tilala,Vishwa Dhinoja, Hetal Pandya and Denish Karia

  • Abstract

    Coumarins have attracted intense interest in recent years because of their diverse pharmacological applications which depends upon the substitution of coumarin. In recent work 4-hydroxy-2Hchromen- 2-one (I) have been prepared by phenol when treated with phosphorus oxychloride and zinc chloride. (I) on further reaction with phosphorus oxychloride and zinc chloride give 4-hydroxy-2- methylenepyrano [3, 2-c] chromen-5(2H)-one (II). Both (I) and (II) when substituted at position-3 are explored for many kinds of biological activity1,2. For this substitution, reaction of (II) has been carried out with acetic acid and phosphorus oxychloride to produce 4-hydroxy-3-methyl-2-methylenepyrano [3, 2-c] chromen-5(2H)-one (III). Reaction of (III) with ethyl acetate and pulverized sodium gives 4- hydroxy-3-(3-oxobutyanoyl) pyrano [3, 2-c] chromen-2, 5-dione (IV). Synthesized compounds have been characterized by UV, IR and NMR.

Synthesis and Biological Screening of Novel Heterocyclic Compounds

Tarunkumar M. Patel and A.M Patel

  • Abstract

    4-(1H-naphtho[1,8-de] [1,2,3]triazin-1-ylsulfonyl)-N-arylidene aniline (2a-e) was synthesised by a facile condensation of aromatic aldehydes with 4-(1H-naphtho[1,8-de] [1,2,3] triazin-1-ylsulfonyl)aniline (1) in good yield. Cyclo condensation of compounds (2a-e) with Succinic anhydride yields 1-(4-(1H-naphtho[1,8- de][1,2,3]triazin-1-yl sulfonyl)phenyl)-5-oxo-2-arylpyrrolidine-3-carboxylic acid (3a-e). The structures of these compounds were established on the basis of analytical and spectral data. All the newly synthesized compounds were evaluated for their antibacterial and antifungal activities.

Excess Molar Enthalpies of mixing of sec- or tert-Butyl chloride with Aromatic hydrocarbons at the temperature 308.15 K

NaveenVerma, Hari Om, Krishan Chander Singh

  • Abstract

    Excess molar enthalpies of mixing for sec- or tert-butyl chloride + benzene or toluene or o- or m- or pxylene have been determined experimentally as a function of mole fraction over the whole composition range at 308.15 K. were measured by a 2-drop calorimeter. The data have been analyzed qualitatively in terms of specific electron donor- acceptor type interactions and the interruption of the molecular order of the pure component in the mixture. The observed data of enthalpies of mixing for these binary mixtures are also analyzed in terms of Flory theory. The Flory theory gave poor agreement between experimental and calculated values.

Spectrophotometeric Determination of Zinc (II) in Food-Stuffs and Biological Samples with Tris-[2, 4, 6-(2-Hydroxy-4-Sulpho-1-Naphthylazo)] -S-Triazine, Trisodium Salt

Sapana Garg, Devender Singh, Sonia Verma and Pratap Singh Kadyan

  • Abstract

    Tris-[2,4,6-(2-hydroxy-4-sulpho-1-naphthylazo)]-s-triazine, tri sodium salt (THT) is proposed as a sensitive and selective reagent for the spectrophotometric determination of zinc(II). An addition of dilute solution of zinc ions to the aqueous solution of THT resulted to form water soluble dark brown complex in the pH range 5.5-7.4, absorbing maximum at 510 nm. The reaction between THT and zinc(II) is instantaneous and the absorbance remains stable for over 24 h. Beer’s law is valid over concentration range 0.0-1.45 ppm with molar absorptivity and Sandell’s sensitivity of 4.75X104 l. mol-1 cm-1 and 0.00145 μg cm-2, respectively. The molar composition of the complex is 1:1 (M:L) as determined by Job’s method of continuous variation. The tolerance limits for interfering ions have been investigated. All variable have been studied in order to optimize the reaction conditions. The efficiency of the proposed method is shown by the successful determination of traces of zinc(II) in food stuffs and biological samples

Purification of Chebulinic Acid from Terminalia Chebula Species by Column Chromatography

Surya Prakash DV, Sree Satya N and Meena Vangalapati

  • Abstract

    Terminalia chebula belongs to the family of Combretaceae. This is used in traditional medicine due to the wide spectrum of pharmacological activities associated with the biologically active chemicals present in this plant. It contains various bio chemical components such as tannins, chebulinic acid, ellagic acid, gallic acid, punicalagin, flavonoids etc. The dried fruits of Terminalia chebula is used to produced the dye. The appearance of dye powder is brown and the main colouring component is chebulinic acid. The objectives of this work were extraction of chebulinic acid from Terminalia chebula by Soxhlet extraction and purify the chebulinic acid by using Column chromatography. From the Soxhlet extraction the chebulinic acid concentration was 6.6 mg/ml and it was increased to 9.4 mg/ml from the Column chromatography. The purity of chebulinic acid was improved by Column chromatography.

Synthesis and Evaluation of Some New Ethoxy- Indole Derivatives as Potential Antimicrobial Agents

B, M.Kalshetty, Ramesh S. Gani, V.M. Chandrasekhar and M.B.Kalashetti

  • Abstract

    The derivatives of indole show biological activities including herbicidal. The newly synthesized compounds methyl-ethoxy indole (Scheme 1), methyl ethoxy indole (Scheme 2) and indole- carboxylic acid ethyl ester (Scheme 3) are for their antibacterial, antifungal, anti inflammatory and analgesics activity. Thus the synthesized drugs are versatile applications in the pharmaceutical and chemical industries. The medical application in the treatment of wounds and tumors. Where the metal complex compounds of triazole, Indole is to impart strength, elasticity and impermeability of water. These drugs of selected metal ions in view of their potential applications in medicinal chemistry, Biotechnology and their structural variety. These drugs are the active component in number of biocides formulations, finding applications in such diverse area as fungicides.

Effect of Temperature on Redox Reactions of α-Hydroxy Acids By Permonosulphuric Acid in Micellar Medium: A Kinetic and Mechanistic Study

P.Rajkumar  and K.Subramani

  • Abstract

    The Oxidation of mandelic acid, lactic acid and glycolic acid by Permonosulphuric acid at 60 ± 0.2°C in micellar medium has been attempted. The reaction is first order kinetics each in PMS and α-hydroxy acids. The rate of electron transfer from α-hydroxy acids to PMS increases with an increase in the concentration of micells and Temperature. It rules out the synchronous C-C bond fission and electron transfer to proton centre. With increase in micells concentration an increase in the rate is observed. The product and stoichiometry corresponds to the reaction of 1 mole of α-hydroxy acids for about 1 mole of PMS. The added CTAB enhances the rate of oxidation of a reaction much more than NaLS

Sensitive Spectrophotometric Determination of Hg (II) in Different Water Samples, Soil Samples and Liver Samples by using 2, 4-Dimethoxybenzaldehydeisonicotinoylhydrazone (DMBHIH)

K. Ramakrishna Reddy, N. Devanna and K.B. Chandrasekhar

  • Abstract

    A rapid, simple, sensitive and selective spectrophotometric method has been developed for the determination of Hg (II) using newly synthesized Chromogenic reagent 2,4-Dimethoxybenzaldehydeisonicotinoylhydrazone (DMBHIH). Hg(II) forms a Yellow coluored water-soluble complex with 2,4- Dimethoxybenzaldehyde isonicotinoylhydrazone (DMBHIH) in the pH range 6.0-10.0. The complex shows maximum absorbance at λmax 390 nm and in the pH range 7.0-9.0. At λmax 390 nm the complex shows maximum absorbance while the reagent blank shows negligible absorbance. Hence, analytical studies are carried out at λmax 390 nm and at pH 8.0 (Phosphate buffer) against reagent blank. Beer's law is obeyed in the range 0.5014-6.0177 mg/mL and the optimum concentration range obtained from ringbom plot is 1.0029-5.0147mg/mL of Hg(II). The molar absorptivity and Sandell's sensitivity for the coloured solution was found to be 2.8x104 L mol-1cm-1 and 0.00571 μg.cm-2 respectively. The interference effect of various diverse ions has been studied. The complex shows 1:1 [Hg(II) : DMBHIH] stoichiometry with stability constant 4.5653x106 obtained from job’s method. The standard deviation of the method in the determination of 1.00295μg ml-1 of Hg(II) is 0.001 and the Relative standard deviation is 1.30 %. First and second order derivative spectroscopic method is developed at λmax 450 nm and 465 nm respectively for the determination of Hg (II), which is more sensitive than the zero order method. The developed method has been used for the determination of Hg (II) in different water samples, soil samples and liver samples. The results are in good agreement with the certified values.

Kinetic Study of Phosphotungustic Acid Catalyzed Oxidation of Benzyl Alcohol by N-Chlorosaccharin in Acetic Acid-Water Medium

H.D. Gupta, S.K. Singh and Santosh Kumar Singh

  • Abstract

    Kinetic investigations in Keggin-type phosphotungstic acid catalyzed oxidation of benzyl alcohol by Nchlorosaccharin, (NCSA) in aqueous acetic acid have been studied. Oxidation kinetics of benzyl alcohol by N-chlorosaccharin in presence of Phosphotungstic acid (PTA) shows a first order dependence on NCSA and fractional order on benzyl alcohol and PTA. The variation of [H+] and [saccharin] (reaction product) have insignificant effect on reaction rate. Activation parameters for the reaction have been evaluated from Arrhenius plot by studying the reaction at different temperature. The rate law has been derived on the basis of obtained dat and a plausible mechanism has been proposed.

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