Rafidain journal of science

Complexes of the type [Cu(B`SCH)(AH)](NO3)2 and [Cu(B`SC)(A)] have been
prepared in neutral and basic mediam, respectively, (where AH= substituted salicylic
acid: salicylic acid-SA and o-acetylsalicylic acid-OASA and 3,5-dinitrosalicylic acid-
DNSA or 5-aminosalicylic acid-ASA or 5-sulphosalicylic acid-SSA; A=deprotonated
form of the AH ligand; B`SCH=benzoin semicarbazone; B`SC=deprotonated form of the
ligand B`SCH).The prepared complexes were characterized by copper ion determination,
relative molecular weight determination, magnetic and molar conductance
measurements, infrared and electronic spectral data.
The effect of γ-rays have been studied on the aqueous solutions of the complexes
under conditions where the hydroxyl radicals were scavenged by 10-3 M sodium formate
in presence of dinitrogen gas at room temperature (25 ± 2 oC). Results indicated that
copper (II) was reduced to copper (I) and a charge transfer between metal ion and ligands
in some complexes were noticed. Some complexes have been completely decomposed
while others did not affect by the radiolysis.

Tin metal react with bis (thiophosphoryl) disulfide in refluxing toluene to give the
compound tetrakis- (o,o′-diethyl dithiophosphate) tin(IV). [Sn{S2P(EtO)2}4], through an
oxidative addition reaction. Tri and pentanuclear complexes of general formulas
[Sn{S2P(EtO)2}4(MCl2)n], and a mixed valance Sn(II) and Sn(IV) compound of general
formula [Sn3{S2P(EtO)2}4Cl4], M=Co(II), Ni(II) or Cu(II),n=2,4 were prepared by a
direct reaction of MCl2.6H2O, (M=Co,Ni), CuCl2.4H2O and SnCl2.2H2O with the tin
compound. The complexes of the general formula [Sn3{S2P(EtO)2}4Cl4(MCl2)2],were
prepared from the reaction of [Sn3{S2P(EtO)2}Cl4] and MCl2.6H2O (M=Co,Ni) and
CuCl2.4H2O. The prepared were characterized by atomic absorption, IR and UV/Vis
spectroscopy, conductivity and magnetic measurments.

A simple and sensitive spectrophotometric method for the assay of sulphadiazine
(SDA) in aqueous medium is described, the method is based on the formation of a yellow
coloured azo dye from the diazotisation of SDA followed by a coupling reaction with
histidine in alkaline medium of sodium hydroxide. The intensity of absorbance for the
resulting yellow azo dye was measured at 423 nm and the azo dye was stable at least for
55 minutes. Beer’s law is obeyed in the concentration range of 10 – 240 μg of SDA in a
final volume of 25 ml, with a molar absorptivity of 1.75×104 L.mol-1.cm-1, a relative error
of +0.34 to +0.44% and a relative standard deviation of ±0.34 to ±0.87%, depending on
the concentration level of SDA.
The method has been successfully applied for the assay of SDA in burn cream and
in a veterinary injectable solution.

Chalcones (1,3-diaryl-2-propen-1-ones) (1-13) were prepared using Claisen-
Schmidt condensation, while Schiff bases (N-arylidene benzylamines) (14-20) were
produced by the condensation of benzyl amine with substituted benzaldehydes. Schiff
bases were added through 1,3-anionic cycloaddition to the double bond of chalcones
under phase-transfer catalysis conditions to afford the corresponding heterocycles
(pyrrolidines 21-30).
Spectral methods were used to support the structures of the new products, while the
suggested mechanisms were investigated depending on the spectral identification as well
as some theoretical parameters such as heat of formation (H.F) and steric energy (S.E).
The biological activity of some reactants and some final products had been tested through
its effects on two kinds of bacteria.

The research was concerned with chemical analysis of the gastric juice in duodenal
ulcer patients caused by Helicobacter pylori infection. The study included (25) patients
(13 males and 12 females) attending endoscopy unit of Salam General Hospital where
gastric juice was taken. Also gastric juice from (25) normal healthy subjects (13 from
males and 12 females) as control were collected for chemical analysis. The chemical
analysis of gastric juice included measurement of electrolytes (Na+, K+, Ca+2 and Cl-)
lactate, glucose, total lipids, iron in addition to conductivity and viscosity. The results of
statistical analysis predicted significant differences in the levels of sodium, chloride, iron,
lactate, glucose and conductivity in gastric juice of duodenal ulcer male patients infected
with H. pylori in comparison to control male. However, potassium, calcium, total lipids
and viscosity showed non significant difference. Females patients, however, showed
significant differences for sodium, iron, calcium, lactate, glucose, total lipids and
viscosity while potassium, chloride and conductivity showed non significant differences
in comparison with healthy females

In the present investigation, some new 1,3,4-oxadiazole derivatives have been
prepared starting from readily available thymol. The reaction of thymol with
ethylbromoacetate afforded the ethyl ester (1). Treatment of the latter with hydrazine
hydrate yielded the corresponding hydrazide (2).
2,5-Disubstituted-1,3,4- oxadiazole (3a-h) were obtained by the reaction of the
hydrazide with substituted benzoic acid in the presence of phosphorous oxychloride.
The structure of the new synthesized compounds were confirmed by spectral and
physical means.

Salicylidene aniline and its substituents form 1:1 charge transfer complexes with the
lanthanide shift reagent Pr(fod)3 in cyclohexane indicated by the observation of a new
band in their U.V. spectra located at longer wavelength (λmax = 430 nm) and with its
low extinction coefficient. The colourless solutions of Schiff’s-bases were changed to
yellow on complexation with Pr(fod)3.
Equilibrium constant values (K) for the complexes were calculated by applying
Benesi-Hildebrand equation at different temperatures, and the thermodynamic parameters
ΔH, ΔS and ΔG were obtained. Negative values of ΔG indicates that the complexation
occurs spontaneously.
Application of Hammet equation on K values for the para substituents show straight
line with negative slope indicating that the electron donating groups enhances the
reaction of complexation.

In the present study we have measured the electrical conductivity of some
potassium halides (KCl, KBr and KI) in methanol at different temperatures (298-318°K).
The conductivity parameters (R, Ka and Λ°) have been calculated by using Lee-Wheaton
equation. The thermodynamic parameters (ΔH, ΔG and ΔS) are also calculated for these
salts.
For the three electrolytes, and at any temperature, it is found that both Λo and Ka
increase with increasing temperature following the order:
Λo KCl < Λo KBr < Λo KI While KaKCl > KaKBr > KaKI The overall distance parameter (R) is
inversely proportional with temperature.

In the present work, the synthesis of some new fused heterocyclic rings derived
from 3-benzofuranone was achieved. 3-Benzofuranone (1) was prepared by the action of
polyphosphoric acid on phenoxyacetic acid. 3-Benzofuranone was treated with
benzaldehyde and furfural in alkaline medium to afford 2-arylidene-3-benzofuranone
(aurones) (2, 3). The reactions of the synthesized aurones with hydrazine hydrate, phenyl
hydrazine, hydroxylamine hydrochloride, acetamide, urea and thiourea gave substituted
pyrazoline (4, 5), 3-phenyl pyrazoline (6, 7), isoxazole (8, 9), 2-pyridinone and
pyrimidin-2-one(thione) (12-15) respectively fused with 3-benzofuran. The structures of
the synthesized compounds were confirmed by IR and physical methods.

An easy and extremely sensitive square wave voltammetric method for the
determination of coenzyme Q10 has been evolved. The method is based on the direct
measurement of the reduction peak current of the coenzyme Q10 at (-0.20 V)[(Ep) versus
the Ag/AgCl reference electrode) at (pH = 7.3) and (25°C). The magnitude of the
reduction peak current (at Ep) has been found to be related to the concentration of the
coenzyme over the range of (8.8 x 10-8 – 5.4 x 10-7 M) (r = 0.9893) and the relative
standard deviation of the method at the (1.3 x 10-7 M) [113 ppb] level is (± 3.9 %) [n
(number of samples) = 6]. The presence of albumin with CoQ10 causes a large depression
in the reduction peak current of the coenzyme and its (Ep) moves to (-0.18 V).

A simple, rapid and sensitive spectrophotometric method for the determination of
sulphacetamide sodium (SAS) was described. The method based on the oxidative
coupling reaction of trifluoperazine hydrochloride (TFP) with SAS using ammonium
ceric sulphate (ACS) as oxidizing agent in acidic medium to form a water soluble
product, that is stable and has a maximum absorption at 560 nm. Beer’s law is obeyed in
a concentration range of 1-22 μg.ml-1 SAS with a molar absorptivity of 7.0×103 L.mol-1
.cm-1, a relative error of –0.56 to +2.33% and a relative standard deviation of ±2.56 to
±4.56% depending on the concentration of SAS. The proposed method has been
successfully applied to the determination of SAS in various ophthalmic preparations

The electrical conductivity of trans – dichloro bis(ethylenediamine) cobalt (III)
chloride [Co(en)2Cl2] Cl has been measured in (methanol + water), (ethanol + water) and
(isoproponal + water) at different percentages and at 298K. The conductivity parameter,
Λo (equivalent conductivity at infinite dilution, Ka; (association constant) and R the
(distance parameter) between the ions were calculated by using Lee – Wheaton equation
for symmetrical electrolytes.
The Walden product (Λ oη ) found to be not constant for the three media which
describe as to the change of ion-solvation and of the solvent structure.

This paper deals with the extraction of a pigment (Malvidin-3-fructoside) from the
Iraqi Kurdistan grape (Vitis vinifera L.). The extracted pigment was purified using
physical methods including different chromatographic techniques (TLC, PC, PTLC and
HPLC). The pure extracted pigment was identified using different techniques such as
infrared (IR), ultraviolet (UV), 1H-NMR, 13C-NMR and CHN analysis.
The isolated pigment from grape was suggested to be very useful indicator for acidbase
titration due to good precision and accuracy compared with commercial indicators
such as methyl orange, methyl red and phenolphthalein. This pigment was also used in
the preparation of indicator paper.