JSCS Vol 67, No. 12
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Impresum |
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J.Serb.Chem.Soc.
67(12)793–802(2002) |
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An optimized synthesis of a key
pharmaceutical intermediate methyl 4-[(1-oxopropyl)phenylamino]piperidine-4-carboxylate
V. D. KIRICOJEVIC, M. D. IVANOVIC, I. V. MICOVIC*, J. B.
DJORDJEVIC**, G.M. ROGLIC* and LJ. DOSEN-MICOVIC*
IHTM-Center for Chemistry,
Njego{eva 12, Belgrade, Yugoslavia,
*Faculty of Chemistry, University of Belgrade, Studentski trg
12-16, Belgrade, Yugoslavia and
**Faculty of Agriculture, University of Belgrade,Nemanjina 6,
11080 Zemun, Yugoslavia
(Received
16 May, revised 26 August 2002)
An
efficient synthesis of methyl
4-[(1-oxopropyl)phenylamino]piperidine-4-carboxylate (7) has been developed,
starting from 1-benzylpiperidin-4-one (1). The compound is a key
intermediate in the synthesis of new generation, highly active narcotic
analgesics, such as remifintanil, as well as the novel classes of fentanyl
analogues. An optimized Strecker-type condensation of piperidone 1 with aniline
and HCN yielded the anilino-nitrile 2(»90 %) which, upon selective
hydrolysis with conc.H2SO4, gave the
anilino-amide 3.After vigorous basic hydrolysis of 3, followed by
acidification and successive treatment with SOCl2and MeOH,
the anilino-ester 5 was obtained (40–45 %, in 3 steps). N-Acylation of 5
with propionyl chloride yielded the anilido-ester6(70–80 %). In the
final step, the catalytic N-debenzylation of6was examined under various
conditions and optimized to yield 7 in near quantitative yields.
Keywords:
optimized Strecker reaction, functionalized piperidines, fentanyl-type
central analgesics.
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J.Serb.Chem.Soc.
67(12)803–808(2002) |
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The effect of solvent on the
kinetics of the oxidation of benzaldehydes by quinolinium chlorochromate
in aqueous organic solvent media
G. FATIMA JEYANTHI, G. VIJAYAKUMAR and K. P. ELANGO
Department of Chemistry, Gandhigram
Rural Institute (Deemed University), Gandhigram 624 302, India, E-mail:
drkpelango@rediffmail.com
(Received
15 May, revised 3 September 2002)
The
kinetics of the oxidation of benzaldehyde and para-substituted benzaldehydes by
quinolinium chlorochromate in water-dimethylformamide mixtures has been studied
under pseudo-first-order conditions at 25±0.2°C. The operation of non-specific
and specific solvent-solute interactions was explored by correlating the rate
data with solvent parameters through a correlation analysis technique. Both
electron-releasing and electron-withdrawing substitutents enhance the rate of
oxidation and the Hammett plot shows a break in the reactivity order indicating
the applicability of a dual mechanism.
Keywords:
kinetics, solvent effect, structural effect, benzaldehyde, oxidation.
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J.Serb.Chem.Soc.
67(12)809–817(2002) |
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Immobilization of Na,K-ATPase
isolated from rat brain synaptic plasma membranes
TATJANA MOMIC, ZORAN VUJCIC*, VESNA VASIC** and ANICA HROVAT
Vinca Institute of Nuclear
Sciences, Laboratory for Molecular Biology and Endocrinology, P. O. Box 522,
YU-11001 Belgrade
*Faculty of Chemistry, University of Belgrade, P. O. Box 158,
YU-11001 Belgrade and
**Vinca Institute of Nuclear Sciences, Laboratory for Physical
Chemistry, P. O. Box 522, YU-11001 Beograde, Yugoslavia
(Received
23 April 2002)
Rat
brain Na,K-ATPase partially purified by SDS from synaptic plasma membranes
(SPM) was immobilized by adsorption on nitrocellulose (NC), polyvinylidene
fluoride (PVDF) and glass fiber (GF) membranes. Partial SDS solubilization
increased the enzyme activity by 40 %. With regard to the preservation of the
enzyme activity, nitrocellulose was shown to be the optimal support for the
immobilization. The enzyme showed the highest percentage activity (14 %) after
30 min of SPM adsorption, at 20°C under the vaccum, with 25 mg of proteins per
NC disc filter. In addition, adsorption on NC stabilizes the Na,K-ATPase, since
the activity was substantial 72 h after adsorption at 20°C. After adsorption,
the sensitivity of the enzyme to HgCl2and CdCll2 inhibition
was higher. The results show that immobilized Na,K-ATPase SPM can be used as a
practical model for the detection of metal ions in different samples.
Keywords:
Na,K-ATPase, synaptic plasma membranes, immobilization, inhibition, cadmium,
mercury.
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J.Serb.Chem.Soc.
67(12)819–824(2002) |
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SHORT COMMUNICATION
Insulin-induced
glycosylphosphatidylinositol (GPI) binding to red cell membrane proteins
NENAD TOMASEVIC, MILAN NIKOLIC and VESNA NIKETIC
Department of Chemistry, University
of Belgrade, Studentski trg 12-16, P. O. Box 158, YU-11001 Belgrade, Yugoslavia,
E-mail address: vniketic@chem.bg.ac.yu
(Received
10 July 2002)
In
this work GPI binding to membrane proteins from erythrocytes of insulinoma
patients for whom prolonged hyperinsulinism and hypoglycemia were
characteristic, as well as from normal erythrocytes incubated with
supraphysiological concentrations of insulin were analyzed. In the RBCs from
insulinoma patients, covalent GPI binding to red cell membrane proteins in the
spectrin/ankyrin region, band 4.1 and two proteins of molecular mass of 115 and
110 kD was demonstrated. In erythrocytes incubated with insulin label was
associated with band 4.1 and two proteins of molecular mass of 115 and 110 kD.
Extraction studies showed that the 100-kD proteins are unrelated to band 3
since they were found in Triton-prepared cytoskeleton. To our knowledge this is
the first demonstration of such a modification of red cell skeletal proteins,
and the first demonstration of post-translation GPI binding to red cell
skeletal proteins in response to insulin. A mechanism proposed for GPI binding
to red cell skeletal proteins as well as the relevance of these results for
physiological disorders that are characterized by hyperinsulinism are briefly
discussed.
Keywords:
insulin; GPI; erythrocytes; membranes; hyperinsulinism; hypoglycemia.
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J.Serb.Chem.Soc.
67(12)825–832(2002) |
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Synthesis and characterization of
Cr(III), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) complexes of
2,12-dimethyl-3-13-di-n-propyl-1,4,11,14-tetraazacycloeicosa-1,3,11,13-tetraene
RAGHU N. PRASAD and MALA MATHUR
Department of Chemistry, University
of Rajasthan, Jaipur-302 004, India, E-mail: prasadraghunandan@yahoo.com
(Received
15 February, revised 26 August 2002)
Metal
complexes of a 20-membered tetraazamacrocycle
2,12-dimethyl-3,13-di-n-propyl-1,4,11,14-tetraazacycloeicosa-1,3,11,13-tetraene
(L) of the type [MLX2]X (M = Cr(III), Fe(III); X = NO3) [CoLNO3]NO3, [NiL(NO3)2], [CuL]Cl2 and [ZnLCl2] have been
prepared by 2 + 2 cyclocondensation of 2,3-hexanedione with 1,6-diaminohexane
in the presence of metal ions as templates. These complexes were characterized
by elemental analyses, conductances, IR and electronic spectra and magnetic
measurements.
Keywords:
Macrocyclic complexes, transition metal complexes, IR spectra, electronic
spectra, magnetic moments.
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J.Serb.Chem.Soc.
67(12)833–842(2002) |
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Dielectric properties of some
cadmium and mercury amino alcohol complexes at low temperatures
MAMDOUH S. MASOUD, AHMED M. HAFEZ*, M. SH. RAMADAN and ALAA E.
ALI**
Chemistry Department, Faculty of
Science, Alexandria University, Alexandria, Egypt,
*Physics Department, Faculty of Science, Alexandria University,
Alexandria, Egypt and
**Physics & Chemistry Department, Faculty of Education
“Damanhour”, Alexandria University, Egypt
(Received
13 March, revised 21 August 2002)
The
dielectric properties of some cadmium and mercury amino alcohol complexes were
studied within the temperature range of 100–300 K at the frequencies of 100,
300 and 1000 kHz. The polarization mechanisms are suggested and the dependence
of both e and tg d on both temperature and frequency are analyzed. The analysis
of the data reveals semi-conducting features based mainly on the hopping mechanism.
Keywords:
amino alcohol complexes, Hg, Cd, dielectric properties.
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J.Sereb.Chem.Soc.
67(12)843–859(2002) |
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Quantitative evaluation of iPP
nucleation in the presence of carbon fibres: induction time approach
ANITA GROZDANOV, GORDANA BOGOEVA-GACEVA and MAURIZIO AVELLA*
Faculty of Technology and
Metallurgy, Rugjer Boskovic 16, Skopje, Macedonia and
*Instituto di Ricerca e Technologia delle Materie Plastiche-CNR,
Via Campi Flegrei 34, Comprensorio Olivetti, Fabricato 70, 80078 Pozzuoli,
(Napoli) Italy
(Received
15 March 2002)
Crystallization
and nucleation behavior in model composites based on iPP and differently sized
carbon fibres have been analyzed in this work. The investigations were
performed in the isothermal regime (120–127°C) using PLM and DSC. The results
were analyzed by applying the Avrami and Muchova-Lednicky methods. It was shown
that the carbon fibre surface acts as a nucleating agent during the
crystallization of the iPP matrix. The highest effect was obtained with the
fibres of PP-compatible size (C-T) related to unsized carbon fibres (C-U). The
induction time,ti, and half-time of crystallization
decreased with increasing carbon fibre content. The energy effect on the thickness
of the critical nucleus decreased in the presence of C-fibres, a fact confirmed
by a decrease in the nucleation parameter Q and the difference energy
parameter Ds(Q
decreased from – 4.96 for iPP to –21.32 for C/iPP model composites, and Ds decreased
from 6.14×10-7 J/cm2for iPP to 1.63×10-7 J/cm2for model
composites). The results of the model composites and their comparison with
published data confirmed that the Muchova-Lednicky method could be successfully
applied for the quantitative evaluation of the nucleation parameters not only
in the temperature range previously suggested (130 – 138°C), but also at lower
crystallization temperatures (Tc = 121–127°C).
Keywords:
polypropylene, carbon fibres, crystallization, nucleacion, kinetics.
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J.Serb.Chem.Soc.
67(12)861–866(2002) |
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The respresentative particle of
copper powder and branching of copper dendrites
K. I. POPOV, N. D. NIKOLIC* and Z. RAKOCEVIC**
Faculty of Technology and
Metallurgy, Karnegijeva 4, P. O. Box 3503, YU-11001 Belgrade,
*ICTM - Institute of Electrochemistry, Njegoseva 12, P. O. Box
473, YU-11001 Belgrade and
**Vinca Institute of Nuclear Sciences, P. O. Box 522, YU-11001
Belgrade, Yugoslavia
(Received
22 July 2002)
Electrochemically
deposited copper powders, which are formed of particles of different size and
morphology, are characterized by some properties like specific surface and
apparent density. A procedure of the determination of a representative powder
particle, exhibiting the same values of specific surface and apparent density
as the powder is proposed. The proposed procedure also permints an explanation
of the branching of copper dendrites.
Keywords:
copper powder, copper particle, representative powder particle, dendritic
branching.
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J.Serb.Chem.Soc.
67(12)867–877(2002) |
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Structure and stereochemistry of
electrochemically synthesized poly-(1-naphthylamine) from neutral acetonitrile
solution
GORDANA CIRIC-MARJANOVIC, BUDIMIR MARJANOVIC*, VOJISLAV
STAMENKOVIC**, ZELJKO VITNIK***, VESNA ANTIC****, and IVAN JURANIC***,
Faculty of Physical Chemistry,
University of Belgrade, Studentski trg 16, P. O. Box 137, YU-11001 Belgrade,
Yugoslavia,
*Centrohem, Karadjordjeva 129, YU-22300 Stara Pazova, Yugoslavia,
**Lawrence Berkeley National Laboratory #I Cyclotron Road, MS
2-100, Berkeley, CA 94720, USA,
***Faculty of Chemistry, University of Belgrade, Studentski trg
16, YU-11001 Belgrade, Yugoslavia and
****Institute for Chemistry, Technology and Metallurgy - Center
for Chemistry, Njegoseva 12, YU-11000 Belgrade, Yugoslavia
(Received
1 February 2002)
Poly-(1-naphthylamine)
films were synthesized potentiodinamically and potentiostatically from
1-naphthylamine in neutral acetonitrile medium using a platinum electrode.
These polymer films were investigated by infrared spectroscopy. Contrary to
earlier published results neglecting the stereochemistry of the
poly-(1-naphthylamine), we predict on the basis of quantum stereochemical
analysis of the possible structural subunits of the polymer, that the ordinary
N–C(4) coupled product is not predominant in the polymer because it is far
removed from the expected planarity. Based on the results of IR investigations
and semiempirical quantum chemical calculations, it is propose that the polymer
products are formed via mixed N–C(4), N-C(5) and N–C(7) coupling routes.
The heats of formation of the oxidized 1-naphthylamine dimers and hexamers were
calculated.
Keywords:
coupling routes, infrared spectroscopy, polymer strcture,
poly-(1-naphthylamine) films, stereochemistry.
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J.Serb.Chem.Soc.
67(12)879–885(2002) |
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Preconcentration method for trace
metals in natural waters using 4-morpholine dithiocarbamate
Z. TODOROVIC, P. POLIC*, T. SABO* and M. CAKIC
Faculty of Technology, University
of Nis, Bulevar Oslobodjenja 124, Leskovac
*Faculty
of Chemistry, University of Belgrade, P.O.Box 158, YU-11001 Belgrade,
Yugoslavia
(Received
15 April, revised 8 August 2002)
The
optimum conditions were found for the preconcentration of trace metals in
natural waters and model samples with standard metals concentrations by using
4-morpholinedithiocarbamate. The formed complexes were extracted with
chloroform. Different methods for recovering the metals from the organic
solvent were studied and compared before AAS metal analysis. The developed
preconcentration method was successfully applied to the determination of trace
metals concentrations in water samples from the “Barje” lake (Leskovac,
Yugoslavia).
Keywords:
preconcentration, chelating extraction, water analysis.
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J.Serb.Chem.Soc.
67 (12)887–892(2002) |
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Residues of atrazine in
agricultural areas of Serbia
S. GASIC, M. BUDIMIR, D. BRKIC and N. NESKOVIC
Institute for Plant Protection and
Environment, T. Drajzera 9, 11000 Belgrade, Yugoslavia
(Received
2 July 2002)
In
this paper the results of a five-year investigation of the pollution of soil,
as well as of surface and groundwater by atrazine are reported. The soil
samples were collected from different localities, from the tillage level, at
two depths (0–15 and 15–30 cm) during the period September-November from 1995
to 1999. The surface and groundwater samples were taken from the same
localities during the same period. The residues were detected by the ELISA
test. The results showed that almost all the analysed soil samples contained
residues of atrazine. These quantities varied from 0.02 to 0.10 mg/kg (0–15
cm), and up to 0.05 mg/kg (15–30 cm), depending on the locality, soil type and
the year of investigation. Concerning the residues in the surface and
groundwater, it was found that most of the analysed samples contained atrazine
residues. In the case of the surface water, the quantity of the residues ranged
from 1.0 to 4.13 mg/L, whill the ground water contained up to 0.3 mg/L
depending on the locality and the year of investigation.
Keywords:
atrazine, soil, groundwater, surface water.
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Subject Index of Vol. 67
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Author Index of Vol. 67
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End of Vol. 67
Copyright & copy; SHD 2003.
Last
Updated January 15, 2003.
For
more information contact: SHD@elab.tmf.bg.ac.yu