Asian Journal of Chemistry

261-267

Authors: H.E. Dinesha and K. Mantelingu*

In present work, an efficient and direct method for the synthesis of hexahydrochromeno[4,3- b]pyrrolo[2,1-a]isoquinolines is reported. This method involves ®T3P mediated oxidation of alcohols to aldehydes followed by [3+2] cycloaddition to afford hexahydrochromeno[4,3-b]-pyrrolo[2,1- a]isoquinolines with good yields

275-278

Authors: N. Agnihotri* , S. Akhtar, P. Rathi and N. Kaur

A simple, fast, selective and sensitive method is developed for the microdetermination of tungsten(VI) with 3-hydroxy-2-[1′-phenyl-3′-(p-methylphenyl)-4′-pyrazolyl]-4-oxo-4H-1-benzopyran (HPMPPB). The reagent forms a 1:4 (M:L) yellow complex in HCl medium which is extractable into chloroform and exhibits maximum absorbance at 415-430 nm. The Beer′s law holds good in tungsten(VI) concentration range of 0.0-2.0 µg mL-1 with molar extinction coefficient and Sandell′s sensitivity of 9.936 × 104 dm3 mol-1 cm-1 and 0.0019 µg W cm-2, respectively at 420 nm . The proposed method is free from the interference of a large number of analytically important elements and shown to give satisfactory results in the analysis of various synthetic and industrial samples of varying composition.

283-286

Authors: S.A. Folane , K.S. Paithankar *, V.B. Deshmukh , U.N. Shelke , S.B. Iyyer and V.K. Gade

The growth mechanism of polyaniline (PANI) and poly(O-anisidine) (POA) with supporting electrolyte HClO4 on indium tin oxide (ITO) substrate has been investigated. The polymer film of PANI and POA deposited on indium tin oxide substrate have been synthesized by electrochemical polymerization method under galvanostatic condition in aqueous solution with supporting electrolyte HClO4 at 27 ºC. To compare the amperometric response of PANI and POA film on aurease enzyme in conventional sensor, the organized materials were characterized by analytical techniques such as UV-visible, FTIR and FE-SEM analyses. The performance of developed sensor was evaluated and the obtained urea biosensor exhibited shorter response time (3 s), wider range 1 × 10-9 to 9 ×10-9 M and the detection limit found to be 1 × 10-9 M. About 80 % of enzyme activity is retained for about 40 days. Modified sensor gives better result by polyaniline than poly(O-anisidine) sensor.

293-296

Authors: Maximus Pranjoto Utomo* , Mohammad Shobirin and Anti Kolonial Prodjosantoso

The compound of β-Ca2SiO4 has been considered as one of the important portand cement components. The existence of metals in the cement raw materials causes β-Ca2-xMxSiO4 formation possibility. The β-Ca2-xZnxSiO4 (x = 0, 0.01 and 0.025) has been prepared and characterized, and aplied for degradation of Congo red. The samples were synthesized by heating stoichiometric amounts of Zn(NO3)2·6H2O, CaCO3 and SiO2 at 950 ºC for 4 h followed by air quenching. The samples were characterized by using XRD, SEM, EDA and UV-visible spectroscopic methods. The XRD patterns indicate that the samples are isomorphous with β-Ca2SiO4. The SEM micrographs depicted the aggregated irregular shape particles having size about 0.2 µm. The EDA measurements revealed that the bulk compositions of materials are as expected. The doping of zinc increases the Eg of the sample and decreases the photocatalytic power for degradation of Congo red under sunlight.

303-308

Authors: S. Hamdiani , I.H. Rohimah , N. Nuryono , A.A. Purwoko , L.R.T. Savalas and S. Hadisaputra*

The corrosion inhibition efficiency of dibenzo-diaza-15-crown-5 (N) and its heterocyclic analogs containing O, S, and P atoms were investigated by ab initio MP2 calculations in aqueous phase. Heteroatoms have a significant role in the corrosion inhibition performance of the studied systems. The geometry parameter shows that the decrease of bond length corresponds to the increase of heteroatom covalent radius. It was revealed that phosphorus more easily donates its electrons to iron than other heteroatoms. Quantum parameters such as high occupied molecular orbital energies (EHOMO) and the fraction of electrons transferred (∆N) have a linear relationship with inhibition efficiencies (IE %). Analysis of second order interaction energies showed the highest back-donation contribution of metal to phosphorus. Theoretical calculations shows that corrosion inhibition increases in the sequence of oxygen < nitrogen < sulfur < phosphorus.

317-320

Authors: Kamal B. Nada , Husam Saleem Khalaf *, Zainab Abbas Hassan Al-Dulaimy , Maha Faisl Ahmed and Azhar Sadiq Hammodi

Stable isotope (δ18O, δD) values were determined along with the chemical compositions at 10 different locations along the Tigris river between Baghdad-Ammara cities of Iraq. The physico-chemical parameters and isotopic data were measured. The sampling site represents 34 % of total Tigris river in the republic of Iraq. The systematically increased in values of stable isotope as move from the downstream of the river and the most significantly appears at Kut lake. This increase occurs as a result of several factors, viz. (a) evaporation occurs low water level in the river and its tributaries, and (b) return flow water to the river from irrigation water in groundwater systems. The change in ion distribution and in the isotopic values related directly with the outcome from the groundwater and sewage station's water.

327-332

Authors: Faiq F. Karam*, Luma Abdalalah Sagban Alabadi and Dunya A. Al-Jibury

In this work, monitoring of monthly variation (from May 2016 to October 2016) in the concentration of the metals (Co, Zn, Cd, Pb, Ni and Fe) from Al-Diwaniya city of Iraq. Investigation about the pollution with these metals was achieved from five selected sites locate in study area by flame atomic absorption spectroscopy. The results showed a wide variation in the levels of heavy metals from site to site and from month to month. A total of 180 surface soil samples were analyzed to detecting the pollution with selected samples. The results showed that the highest concentration with Ni was 6.290 mg kg-1 while the lowest concentration detected with Ni was 0.080 mg kg-1. The results of pollution index (enrichment factor, contamination factor, pollution load index and geo-accumulation) of heavy metals (Co, Zn, Cd, Pb, Ni) had the following order: Zn > Cd > Ni > Pb > Co.

337-342

Authors: Duy Trinh Nguyen , Thuong Nhan Phu Nguyen , Duy Chinh Nguyen, Van Thi Thanh Ho , Md. Rafiqul Islam , Kwon Taek Lim and Long Giang Bach*

An effortless and efficient method for the alteration of SiO2 nanoparticles by poly(2-hydroxyethylmethacrylate) (PHEMA) has been developed. Initially, a strategic atom transfer radical polymerization (ATRP) initiator was anchored to SiO2 nanoparticles surface via coupling reaction followed by surface-initiated atom transfer radical polymerization of HEMA successfully afforded chemically grafted PHEMA to SiO2 nanoparticles (PHEMA-g-SiO2). We used XPS, FT-IR and EDS analyses for confirming the covalent immobilization of PHEMA onto SiO2 nanoparticles. TGA/DSC and zeta potentials measurements were used for determining the thermal and surface charge features of the nanocomposites, respectively

348-352

Authors: Ashok S. Pise *, Arvind S. Burungale , Santosh S. Devkate , Ramesh B. Gawade and Sunil D. Jadhav

The α,β-unsaturated cyanoester was obtained from p-methoxy benzaldehyde and ethyl cyano acetate by reported method. The conjugated addition products were synthesized from alkyl or aryl bromides and α,β-unsaturated cyanoester in the presence of 10 mol % Cu(I) catalyst in high yields within 17-21 min under ultrasound irradiation.

360-366

Authors: Gubran Alnaggar, K.R. Raksha and S. Ananda*

Monoclinic molybdenum dioxide (MoO2) nanosheets have been successfully synthesized by a simple electrochemical method. The as prepared MoO2 was used as a photocatalyst for the photocatalytic degradation of Indigo carmine dye under various experimental conditions and also as oxygen evaluation catalyst for the decomposition of potassium permanganate. Initially, as-prepared MoO2 was characterized by different techniques namely, X-ray diffraction, scanning electron microscopy FE-SEM, UV-visible and FT-IR techniques, so as to study and revealed the morphological, structural, functional and optical properties. The results revealed that photocatalyst has nanosheets morphology with thickness less than 10 nm and it has also monoclinic crystal structure with an average crystallite size of 27 nm. The optical properties studies showed that band gap (Eg) value of MoO2 (3.85 eV) lies in the UV region and can be a suitable candidate for UV light photocatalytic application. In addition, the experimental results revealed an excellent photocatalytic performance of MoO2 in the degradation of Indigo carmine under UV light irradiation and also for the decomposition of KMnO4 by oxygen evaluation reaction

373-377

Authors: Chinnadurai Anbuselvan

A green, one-pot three-components reaction of (E)-1-(4-(difluoromethoxy)-2-hydroxybenzylidene) semicarbazide has been designed, synthesized and characterized by elemental, FT-IR, 1 H and 13C NMR spectral data. The cytotoxic activities of the synthesized compound were evaluated by MTT assay in human cancer cell lines. Docking studies of 3-substituted indolin-2-one scaffolds on vascular endothelial growth factor receptor 2 (VEGFR-2) involved in cell proliferation and angiogenesis was performed. Based on the ligand efficiency indices, Schiff bases may be regarded as efficient candidates for further molecular developments of anticancer agents. The molecule is useful in sensing and drug-carrying applications.

385-388

Authors: Prachi , Asifa Mushtaq and Devendra Singh Negi*

This work reports the synthesis of zinc oxide nanoparticles using leaf extract of Rubia cordifolia, characterization and the antibacterial activities against selected pathogenic bacteria. X-ray diffraction showed that the particle are hexagonal wurtzite in nature and average crystallite size is 23.61 nm. The SEM image revealed that the particles are sheets in shape. TEM image indicates that the size is found in the range of 23.45 nm. Further, as-formed zinc oxide nanoparticles revealed significant antibacterial activity against gram negative Pseudomonas aeruginosa and Escherichia coli and gram positive Micrococcus luteus, Staphylococcus aureus and Streptococcus pneumonia bacterial strain. The current investigation demonstrates convenient consumption of Rubia cordifolia leaf extract as a fuel for the synthesis of zinc oxide nanoparticles through green synthesis method to attain significantly antibacterial activity

393-395

Authors: Alaa K.H. Al-Khalaf*, Karar Abdali , Abdulazeez Obeid Mousa and Muna Aoudah Zghair

Two ligands have been synthesized from hydrazine and benzidine derivatives. These ligands were mixed with metal ions such as [Cd(II) and Zn(II)] to synthesize liquid crystalline complexes. By using polarizing optical microscopy, these compounds have a liquid crystalline behaviour. The complexes were characterized by physical and chemical techniques such as spectroscopic (UV-visible, FT-IR, X-ray powder diffraction) and molar conductivity. The results show enantiotropy nematic phase (marble and schleiren textures through heating and cooling, respectively) for all compounds. Compounds have polycrystalline amorphous structure with square planar geometry

403-409

Authors: H.E. Dinesha , N.C. Sandhya and K. Mantelingu*

An efficient and direct method for the synthesis of tetrahydro-2H-oxazolo[2,3-a]isoquinolines is reported. This novel method involves ®T3P mediated in situ oxidation of benzyl alcohols to aldehyde followed by acetic acid mediated [3+2] cycloaddition reaction to afford tetrahydro-2H-oxazolo[2,3- a]isoquinolines in one-pot operation with good to excellent yields. Heterocyclic alcohols also underwent the reaction with tetrahydroquinolines at room temperature.

417-421

Authors: V. Natchimuthu*, S. Ravi and J. Amoros

Lennox-Gastaut type of seizures that affects the central nervous system (CNS) are facing drug administration problems. One such problem is that the delivery mechanism of antiepileptic drugs (AEDs) to the affected seizures is haunting the complete treatment of epilepsy. One of the better methods to overcome this problem is to attach the drug with a carrier agent and making it deliver at the proper site. In this paper, a novel attempt has been made to identify all possible attachment portions in the antiepileptic drugs like topiramate, carbamazepine and lamotrigine by sonicating (ultrasonic) the drugs at different timings and amplitudes. The disintegration of the drugs and the possible attachment points, for every different timing and amplitude, were analyzed through high performance liquid chromatography. An extensive study has been made on topiramate by reacting it with the chosen drug delivering agent perfluorodecalin (PFD) and subjected to sonication. The choice of perfluorodecalin is a novel intuition since they are traditionally used as oxygen carrier and blood substitute. The topiramate + perfluorodecalin emulsion is grown into a crystal. Complete structure has been elucidated through X-ray crystallographic studies. Results show that the sonication is one of the much easier and handy technique to break chemical bonds and to create cavitations thus allowing other molecules to occupy that space. Investigation further reveals that, more the number of nitrogen atoms, less they are interactive and less it responds to sonication effect. Hence we prefer to safely conclude that topiramate is more adaptive in the study of drug delivering mechanism though it possesses a bulk structure than lamotrigine and carbamazepine.

427-432

Authors: Nor Asiken Abdul Wahab , Mohd Sani Sarjadi , Sazmal Effendi Arshad , Mashitah Mohd Yusoff and Md Lutfor Rahman*

Ion imprinted polymers (IIPs) draw great attention in various fields because of powerful selectivity to the target metal ions. Thus, the synthesis of copper-ion imprinted polymer (Cu-IIP) was performed by using copper ion and complexing agent rufigallol with ethylene glycol dimethacrylate (EGDMA) and 2,2-azobisisobutyronitrile (AIBN). Aqueous HCl was used to leach Cu2+ ions from the imprinted polymer for creation of cavities of template, which is utilized for cooper ions adsorption with high selectivity. The IIP were characterized using ICP-MS, FE-SEM and also solid state analysis by UV-visible NIR spectroscopy. FT-IR study confirmed the successful complexation of Cu-IIP. The optimum pH was found to be 6 and highest adsorption capacity was estimated about 112.5 mg g-1. Thus, IIP gave good selectivity to copper ions in presence of other transition metals and also IIP can be regenerated for eight times without a subst-antial loss in adsorption capacity

438-444

Authors: Ts. Ramishvili*, V. , I. Ivanova , N. Kokiashvili , T. Bukia and G. Kurtsikidze

The geraniol conversion reaction was initiated by the simultaneous action of micro- and micro-mesoporous BEA-type zeolites and ultrasonic irradiation (UMR-300B hybrid reactor, 25 kHz, 100-900 W; SRF-1, 20-60 kHz, 100 W). Geraniol by ultrasonic irradiation at 27-100 ºC, had a low degree of conversion, upto 2 %. Geraniol was a resistant to ultrasound in argon atmosphere solutions of N,N-dimethylformamide and methanol. In methanolic solution, geraniol was actively converted to linalool and to methyl ethers of linalool and nerol with the selectivity of 80 % on zeolite BEA-25 under ultrasonic irradiation in air at 30 ºC. Using BEA-type zeolite/ultrasonic-assisted reaction was increased the degree of conversion of geraniol, the selectivity and yield to linalool and nerol on the most active RBEA-25 zeolite by prolonged ultrasonic irradiation (1.5-5 h) or under combined ultrasound and microwave irradiation (US 300 W/MW 550 W, 1.5 h, 80 ºC)

449-452

Authors: In-Chang Choi and Heon Chang Kim*

Carbon dioxide was directly decomposed by a transferred DC thermal plasma and the effects of plasma induced current on the decomposition efficiency were investigated. The thermal plasma system was operated in a way that the metal oxide particles could be simultaneously produced from an anodic bulk metal (Zn) placed on a carbon crucible, so as to continuously consume atomic and molecular oxygens (O and O2) generated from the CO2 decomposition. As the induced current increased from 120 to 160 A by 20 A, the decomposition efficiency increased almost linearly from 53 to 68 %. The amount of ZnO particles produced from the bulk also increased and the particle crystallinity was improved. Although the concentration of carbon monoxide in the effluent was sharply increased at 160 A, further destruction can be done by re-circulating the effluent to plasma chamber

460-462

Authors: Judy Perez, Chien-Chang Shen and Consolacion Y. Ragasa*

Chemical investigation of the dichloromethane extracts of the mangrove, Exoecaria agallocha Linn. has led to the isolation of alkyl ferulates (1), lupeol (2), a mixture of 3-epi-α-amyrin (3) and 3-epi-βamyrin (4) in about 2:3 ratio, and agallochaol K (5) from the bark; taraxerol (6), epi-taraxerol (7) and chlorophyll a from the leaves; and a mixture of compounds 3 and 4 in about 1:2 ratio, squalene, olean12-en-3-one (8) and fully epoxidized linoleic acid from the twigs. The structures of compounds 5 and 7 were elucidated by extensive 1D and 2D NMR spectroscopy and confirmed by comparison of their NMR data with those reported in the literature. The structures of the other compounds were identified by comparison of their NMR data with literature data.

469-471

Authors: V. Lalitha , T. Maruthavanan and P. Venkatesan*

A simple procedure using grinding method of condensation of N-acetyl-3-methyl-2,6-diarylpiperidin4-one with aldehyde gave N-acetyl-3-arylidene-5-methyl-2,6-diarylpiperidin-4-one with good yield. The structure of the synthesized compounds was assigned on the basis of IR, 1 H NMR and mass spectral studies. The synthesized compounds showed remarkable in vitro antioxidant activity.

477-480

Authors: T. Gomadurai* , K. Rajasekar* , S. Balasubramaniyan, R. Selvarani, C. Veeravel and R. Geetha

The Co(II) and Ni(II) transition metal complexes with benzimidazole and benzoate ion was synthesized using microwave heating. The synthesized complexes were characterized by elemental analysis, metal estimation, molar conductance, cyclic voltammetry, magnetic moment and electronic spectra, IR, FarIR spectral data. The structure and metal ligand stoichiometry of the synthesized complexes were confirmed by using elemental analysis and metal estimation. Molar conductance of 10-3 M complex solution confirming their non-electrolyte nature. The Redox behaviour of metal ions in the synthesized complexes was confirmed by cyclic voltammogram. Six coordinated geometry of complexes were concluded from magnetic moment and electronic spectra. The in vitro antibacterial activities of the ligand and its Co(II) and Ni(II) complexes were screened against Gram +ve bacteria, Bacillus, Gramve bacteria, Pseudomonas, Klebsiella pneumonia and Proteus and in vitro antifungal activities were screened against pathogenic yeast, C. albicans by agar well diffusion method. The antipyretic activities of ligand and its Ni(II) complex were evaluated by yeast- induced fever test. The percentage reduction of the sample at yeast induced temperature was deduced.

487-492

Authors: Lukman Noerochim*, Eriek Aristya P. Putra , Diah Susanti , Firman Mangasa Simanjuntak , Tubagus Noor Rohmannudin and Achmad Subhan

α-Fe2O3 with nano ellipse structure was successfully synthesized by one-step hydrothermal method with adding 3, 6, and 9 mmol glycine at 160 °C for 10 h. FE-SEM images present that the shape and size of α-Fe2O3 is nano ellipse with dimensions in the range length of 130–200 nm and in the range diameter of 77–120 nm. The as-prepared α-Fe2O3 nano ellipse with the addition of glycine by 6 mmol exhibited excellent cycling performance and rate capability when used as anode for lithium ion batteries, obtaining reversible discharge capacity of 206.75 mAh g-1 at 0.3 C. This is attributed to the nano ellipse structure delivering a large particle surface area thus increasing the electric and ionic conductivity of the α-Fe2O3 particles as anode. This result demonstrates that α-Fe2O3 nano ellipse could be a good candidate as anode material for lithium-ion battery.