JSCS Vol 64, No. 2

 

J. Serb. Chem. Soc. 64(2) 83-89 (1999)
UDC 547.586.2:665.652.4
JSCS-2625  
Original scientific paper

Benzylation of N-benzyl-2-phenylacetamide

DUSAN Z. MIJIN, BILJANA M. BOZIC, VIDA D. JANKOVIC, DUSAN G. ANTONOVIC, NADEZDA D. STOJANOVIC and SLOBODAN D. PETROVIC

Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, P.O.Box 35-08, YU-11001 Belgrade, Yugoslavia

(Received 21 April, revised 13 November 1998)
N-Benzyl-2-phenylacetamide was used as a model for the study of the alkylation of N-substituted 2-phenylacetamides with benzyl chloride in the presence of powdered KOH. The reactions were carried out in the presence and absence of phase-transfer catalysts, in order to establish any possible difference in the reaction products. Various phase-transfer catalysts, solvents and temperatures were used. A comparative study with the benzylation reaction of other N-substituted-2-phenylacetamides is presented. The observed lower reactivity of N-benzyl-2-phenylacetamide in comparison with the reactivity of N-ethyl-2-phenylacetamide and N-phenyl-2-phenylacetamide can be explained in terms of steric and polar effects.

Key words: alkylation, N-alkylation, C-alkylation, O-alkylation, N-substituted 2-phenyl-acetamides, phase-transfer catalysis.


J. Serb. Chem. Soc. 64(2) 91-95 (1998)
UDC 547.631.2/.638.1:615.779
JSCS-2626
Original scientific paper

Synthesis and biological activity of some novel fluorenone-, 2- or 7-nitrofluorenone-1-carbonylamino acid derivatives

S. A. M. SHEDID and H. M. HASSAN

Chemistry Department, Faculty of Science, Al-Azhar University, Nasr City, Cairo, Egypt

(Received 15 July 1998)
The synthesis of fluorenone-, 2- or 7-nitrofluorenone-1-carbonylamino acid methyl ester and hydrazide derivatives IV-XXX is described. Many of the products were found to be active against a number of microorganisms. The spectral data of the synthesized compounds IV-XXX and the results of biological screening are briefly discussed.

Key words: fluorenone-1-carboxylic acids, amino acids, biological activity.


J. Serb. Chem. Soc. 64(2) 97-108 (1999)
UDC 661.888.1/547.74/.75:691.16
JSCS-2627
Original scientific paper

Vanadyl porphyrins in sedimentary kerogens/asphaltenes: Estimation of the concentration

PAVLE I. PREMOVIC, THIERRY ALLARD*, NIKOLA D. NIKOLIC, IVANA R. TONSA and MIRJANA S. PAVLOVIC**

Laboratory for Geochemistry and Cosmochemistry, Department of Chemistry, Faculty of Science, University of Nis, P.O.Box 91, YU-18000 Nis, FR Yugoslavia,
*Laboratoire de Mineralogie-Cristallographie, Universit‚s de Paris VI et VII, Place Jussieu - 75252 Paris Cedex 5, France, and
**Institute of Nuclear Sciences Vinca, P.O.Box 522, YU-11001 Belgrade, FR Yugoslavia

(Received 2 November 1998)
A new, rapid method for determining the concentration of vanadyl porphyrins (VO2+-P) associated with the kerogen of bituminous sedimentary rocks, using electron spin resonance (ESR) is described. The method is simple, straightforward and inexpensive. Several concentrations of a vanadyl (VO2+) standard dissolved in glycerol/lignite mixture were prepared. The VO2+ concentrations ranged from 100-1000 ppm. The anisotropic ESR spectra of both the standards and kerogen samples were recorded at room temperature and the integrated areas of the pre-selected ESR line (attributed to nuclear spin mI= -5/2) were computed. The concentrations of VO2+ found in the kerogen samples were calculated using the relative ratio of the integrated areas for the standards and the kerogen samples. The VO2+-P concentrations of the kerogen materials were then calculated using 450 as the mean molecular weight of these species. The quantitative determination of VO2+-P in the kerogen fractions in the range 800 ppm and 8000 ppm and higher is feasible by the method reported. The method of analysis was also extended to asphaltene samples (enriched with VO2+-P) and a coal sample containing non-porphyrin VO2+ associated with its organic fraction.

Key words: vanadyl porphyrins, kerogen, estimation, concentration.


J. Serb. Chem .Soc. 64(2) 109-116 (1999)
UDC 547.815.1-002.61
JSCS-2628
Original scientific paper

The influence of temperature and inorganic salts on therheological properties of xanthan aqueous solutions

KATARINA JEREMIC*, SINISA MARKOV**, BRANISLAV PEKIC* and SLOBODAN JOVANOVIC*

*Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, P.O. Box 35-03, YU-11000 Belgrade and
**Faculty of Technology, University of Novi Sad, YU-21000 Novi Sad,Yugoslavia

(Received 28 October, revised 3 December 1998)
The rheological properties of xanthan gum in aqueous saline solutions and at increased temperatures are of great practical interest especially for its application in enhanced oil recovery during which the xanthan solutions are exposed to increased salt contents and relatively high temperatures. In this work, the influence of high temperature and high salt concentrations (up to 10 mass%) on the rheological properties of xanthan was investigated. The influence of three different salts was examined - NaCl, CaCl2 and FeCl3. Five xanthan samples were used with the goal of comparing their rheological properties. Four of the samples were synthesized in the laboratory of one of the authors and one of them was a commercial sample (BAROID) used for enhanced oil recovery. The viscosity flow curves were determined for the investigated xanthan solutions and the obtained results showed that the rheological behavior of the laboratory prepared xanthan samples was very similar to the rheological behavior of the commercial sample. The investigated inorganic salts at concentrations as high as 10 mass% did not influence the viscosity of the xanthan samples, except Fe3+ ion. Temperature had almost no influence on the viscosity in the investigated interval, especially at the higher shear rates. The shear dependent activation energies of viscous flow were calculated.

Key words: xanthan solution, rheologicaal properties, influence of salt content and temperature.


J. Serb. Chem .Soc. 64(2) 117-122 (1999)
UDC 546.137/546.41'46''47'''/:541.133
JSCS-2629
NOTE

N O T E
Electric conductivity of gel-polymeric electrolytes with Ca, Mg and Zn perchlorate salts

NIKOLA CVJETICANIN and SLAVKO MENTUS

Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, P.O. Box 137, YU-11001 Belgrade, Yugoslavia

(Received 26 June, revised 11 November 1998)
The gel-polymeric electrolytes were prepared with calcium, magnesium and zinc perchlorates dissolved in propylene carbonate together with poly (acrylo nitrile) or poly(methyl methacrylate) as a solution immobilizing polymers. The electric conductivity of these electrolytes was examined in the dependence of temperature and solvent content, at a constant salt-to-polymer concentration ratio. The electrolyte compositions were outlined having the conductivity close to 10-3 S cm-1. It was demonstrated that among the factors determining the conductivity, the cation nature plays a minor role, while the dominant role plays a liquid solvent (propylene carbonate) concentration.
Key words: gel-polymeric electrolytes, perchlorates, electric conductivity.


J. Serb. Chem. Soc. 64(2) 123-130 (1999)
UDC 546.742:541.428.49-541.572.54/
JSCS-2630
Original scientific paper

Thermal investigation of some chelate Ni(II) complexes

NEVENKA RAJIC, DJORDJE STOJAKOVIC and ROMAN GABROVSEK*

Faculty of Technology and Metallurgy, University of Belgrade, YU-11000 Belgrade, Yugoslavia and
*National Institute of Chemistry, Ljubljana, Slovenia

(Received 27 October 1998)
Several diamine-nickel(II) complexes have been prepared and the kinetic parameters of their decomposition reactions investigated. The complexes undergo a gradual thermal decomposition. First, water is lost, followed by the departure of the diamine ligands. The activation energies for the first deamination decrease in the order Ni(1,2-pd)3Cl2(H2O)2 › Ni(en)3Cl2(H2O)2 >> Ni(1,3-pd)3Cl2(H2O)2 >> Ni(dieten)2Cl2 (H2O)2 (en = 1,2-diaminoethane; 1,2-pd = 1,2-diaminopropane; 1,3-pd = 1,3-diaminopropane; dieten = 2-diethylaminoethylamine) which is in accordance with the chelate effect. The decomposition of the complexes can be represented by a variety of solid state decomposition models depending on the particular complex, as well as on the stage of the decomposition.

Key words: nickel(II) complexes, kinetic parameters, activation energy, thermal analysis, TG/DTG-DSC.


J. Serb. Chem. Soc. 64(2) 131-140 (1999)
UDC 661.846/549.6-002.61/
JSCS-2631
Original scientific paper

Physico-chemical characteristics of sepiolites from Golesh

MARINA RADOJEVIC, MIROSLAVA DOJCINOVIC, DANA SIMIC, VERA VUCELIC and OLGICA KOVACEVIC

Institute of General and Physical Chemistry, P.O.Box 551, Studentski trg 12, YU-11000 Belgrade, Yugoslavia

(Received 14 October 1998)
The physico-chemical characteristics of sepiolite from the Golesh deposit (south Serbia), have been investigated by means of SEM, XRD, IR spectroscopy, DTA-TG, the BET method and classical chemical analysis. The textural characteristics of the investigated samples are related to the content and crystallinity of the sepiolite, as well as to the content of magnesite, which can reach up to 40%. The thermal characteristics and IR spectra are typical of sepiolite mineral, accompanied by magnesite.

Key words: sepiolite, Golesh, SEM, XRD, DTA, TG, BET, IR, chemical analysis.


J. Serb. Chem. Soc. 64(2) 141-147 (1999)
UDC 547.475.2:543.432/547.632.6/
JSCS-2632
Original scientific paper

Kinetic determination of ascorbic acid in pharmaceuticalsamples

S. S. MITIC, G. Z. MILETIC, S. M. MILETIC and D. A. KOSTIC

Department of Chemistry, Faculty of Philosophy, University of Nis, YU-18000 Nis, Yugoslavia

(Received 21 October, revised 27 November 1998)
A kinetic method is described for the determination of ascorbic acid based on its inhibiting effect on the Mn(II) catalysis of the oxidation of Malachite Green with potassium periodate. The sensitivity of the method is 35.4 ng cm-3. The relative error ranges between 2.66 and 7.45% for the concentration interval 35.4 to 354 ng cm-3. Kinetic equations are proposed for the investigated process. The effects of certain foreign ions upon the reaction rate were determined for the assessment of the selectivity of the method. The method was applied for the determination of ascorbic acid in pharmaceutical samples.

Key words: kinetic method, ascorbic acid determination, Malachite Green oxidation, pharmaceutical samples.


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