Antimalarial activity of n(6)-substituted adenosine derivatives (part 2)

We have investigated the in vitro antimalarial activity of a new series of adenosine derivatives. The results show that N(6)-(1-naphthylmethyl)-5'-deoxy-5'-(amido)adenosines as well as N(6)-(4-phenylbenzyl)-5'-deoxy-5'-(amido)adenosines display significant activity against the malaria-causing parasites, with the sterically demanding bisubstituted species reported being active in most cases in the low-micromolar range. The novel compounds with unusual substitution pattern were obtained applying an efficient convergent polymer-assisted solution-phase (cPASP) synthesis protocol. Thus, we were able to prepare a series of substituted derivatives in parallel that would have been difficult to synthesize by standard techniques. The scope and limitations of the synthetic methodology are discussed.     

Microdetermination of chlorine and bromine in some organic compounds by ion-selective electrodes

Summary The solid state ion-selective chloride and bromide electrodes are used for the microdetermination of chlorine and bromine in organic compounds. After combustion in an oxygen-filled flask, potentiometric titration with silver nitrate at pH 5–7 in presence of 50% dioxan is carried out. Results accurate to ±0.3% absolute are obtained with some partially and highly halogenated compounds.

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Mikrobestimmung von Chlor und Brom in einigen organischen Verbindungen mit Hilfe von ionenselektiven Elektroden

Zusammenfassung Chlorid- und bromidselektive Festkörperelektroden wurden zur Chlor- und Brombestimmung in teilweise bzw. hochhalogenierten organischen Verbindungen benutzt. Nach Verbrennung im Sauerstoffkolben erfolgt eine potentiometrische Titration mit Silbernitrat bei pH 5–7 in Gegenwart von 50% Dioxan. Die erhaltenen Ergebnisse sind auf ±0,3 % genau.

     

Resorcinol - formaldehyde adsorption of cesium from Hanford waste solutions

Batch equilibrium measurements were conducted at 25±2 °C with a granular resorcinol-formaldehyde (RF) resin to determine the distribution coefficients (K _d ) for cesium. In the tests, Hanford Site actual waste sample containing radioactive cesium (¹³⁷Cs) and a pretreated waste sample that was spiked with non-radioactive ¹³³Cs were used. Initial concentrations of non-radioactive cesium in the waste sample were varied to generate an equilibrium isotherm for cesium. Majority of the tests were conducted at 25±2 °C using a liquid to solid phase ratio of 100 ml/g and at a contact time of 72 hours. Two additional tests were conducted at a liquid to solid phase ratio of 10 and at contact time of 120 hours. The measured distribution coefficient (K _d ) for radioactive cesium (¹³⁷Cs) was 948 ml/g, the K _d for non-radioactive cesium (¹³³Cs) was 1039 ml/g. The K _d for nonradioactive cesium decreased from 1039 to 691 ml/g with increased initial cesium concentration from 8 to 64 g/ml. Very little change of the K _d was observed at initial cesium concentration above 64 g/ml. The maximum sorption capacity for cesium on granular RF resin was 1.17 mmole/g dry resin. This value was calculated from the fit of the equilibrium isotherm data to the Dubinin-Radushkevich equation. Previously, a total capacity of 2.84 mmole/g was calculated by Bibler and Wallace for air-dried RF resin.This work was conducted at the Savannah River Technology Center in Aiken, SC, which is operated for the U. S. Department of Energy (DOE) by Westinghouse Savannah River Company under Contract DE-AC09-96SR18500. The Hanford River Protection Project-Waste Treatment Plant (RPP-WTP) funded this work. The authors are very grateful to Karen Palmer, Betty Mealer, and Yvonne Simpkins for their assistance in the experimental work.     

Microdetermination of phosphorus in organic compounds by indirect spectrophotometric reactions

Summary Organo phosphorus compounds are decomposed by closed-flask combustion. The phosphate ions produced are then converted to phosphomolybdic acid and extracted withiso- butyl acetate. The 12molybdate ions associated with each original phosphate ion are spectrophotometrically determined by reactions with alkaline hydrogen peroxide, hydrogen peroxide and benzidine and gallic acid. The colours are measured at 450, 400 and 400nm respectively.

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Zusammenfassung Organische Phosphorverbindungen werden im Schöniger-Kolben mineralisiert. Das Phosphat wird zu Phosphormolybdänsäure umgesetzt, miti-Butylacetat extrahiert und dann spektrophotometrisch bestimmt. Dazu bedient man sich der Reaktionen mit alkalischem Wasserstoffperoxid, mit Wasserstoffperoxid und Benzidin oder mit Gallussäure. Die Messungen erfolgen bei 450 nm im ersten Fall, bei 400 nm im Fall der beiden letztgenannten Farbreaktionen.

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This paper is taken from the Master's Thesis of S. A. I. Thoria.     

Spectrofluorimetric study of host-guest complexation of ibuprofen with beta-cyclodextrin and its analytical application

The characteristics of host-guest complexation between beta-cyclodextrin (beta-CD) and two forms of ibuprofen (protonated and deprotonated) were investigated by fluorescence spectrometry. 1:1 stoichiometries for both complexes were established and their association constants at different temperatures were calculated by applying a non-linear regression method to the change in the fluorescence of ibuprofen that brought about by the presence of beta-CD. The thermodynamic parameters (deltaH, deltaS and deltaG) associated with the inclusion process were also determined. Based on the obtained results, a sensitive spectrofluorimetric method for the determination of ibuprofen was developed with a linear range of 0.1-2 microg ml(-1) and a detection limit of 0.03 microg ml(-1). The method was applied satisfactorily to the determination of ibuprofen in pharmaceutical preparations.     

Synthesis and Characterization of Novel Monoazo N‐Ester‐1,8‐Naphthalimide Disperse Dyestuffs

Five novel monoazo disperse dyestuffs based on N‐ester‐1,8‐naphthalimide were synthesized. Acenaphthene was nitrated, then oxidized to 4‐nitro‐1,8‐naphthalic anhydride. 4‐Nitro‐1,8‐naphthalic anhydride was reacted with methyl and ethyl glycinate in alcoholic media, followed with reduction. 4‐Amino‐N‐methyl and ethyl glycinate‐1,8‐naphthalimide were obtained. These products were diazotized and coupled with appropriate aromatic amines to give bluish‐red or violet dyestuffs. All intermediates and dyestuffs were purified and characterized by ¹H‐NMR, FTIR, DSC, UV‐VIS and Elemental Analysis. Dispersion of dyestuffs was prepared in water and applied to polyester fabrics. The dyed fabrics showed that four of the synthesized dyestuffs were suitable for coloring polyester fibers, producing deep bluish red with very good build up properties.     

Composition-controlled synthesis of bimetallic gold-silver nanoparticles

This paper reports findings of an investigation of the synthesis of monolayer-capped binary gold-silver (AuAg) bimetallic nanoparticles that is aimed at understanding the control factors governing the formation of the bimetallic compositions. The synthesis of alkanethiolate-capped AuAg nanoparticles was carried out using two related synthetic protocols using aqueous sodium borohydride as a reducing agent. One involves a two-phase reduction of AuCl(4)(-), which is dissolved in organic solution, and Ag(+), which is dissolved in aqueous solution. The other protocol involves a two-phase reduction of AuCl(4)(-) and AgBr(2)(-), both of which are dissolved in the same organic solution. AuAg nanoparticles of 2-3 nm core sizes with different compositions in the range of 0-100% Au have been synthesized. The two synthetic routes were compared in terms of bimetallic composition and size properties. Our new findings have allowed us to establish the correlation between synthetic feeding of metals and metal compositions in the bimetallic nanoparticles, which have important implications to the exploration of gold-based bimetallic nanoparticles for constructing sensing and catalytic nanomaterials.     

Theoretical study of the reaction of alkynes with furan catalyzed by AuCl3 and AuCl

A general scheme for the endo‐ and exo‐cyclization of furan reactivity with [L ‐Au^{III, I}Cl_x] with (x = 3, 1 and L ‐acetylene and vinylidene) complexes is investigated using density functional theory (DFT) code. Two conceivable mechanisms via a [4 + 2] Diels–Alder process or carbene complex are analyzed. According to the activation energy values of the gold (III and I) catalyst, the first mechanism, which implies the Diels–Alder reaction of Au^III, is thermodynamically favored and gives more evidence of the intramolecular addition of the furan with the alkynes. The second mechanism, presumably assisted by the spontaneous formation of the exo‐vinylidene complexes and intermediates of gold (III, I) by forming the carbene complex, is kinetically favored. Additionally, we compare our results with other structures with intramolecular additions that exhibit the quasi‐similarity of gold analogue structures. Differences in activation energies are observed, according to the functional used. Finally, we probe the solvent effects, which decrease the energy barrier in the path. © 2006 Wiley Periodicals, Inc. Int J Quantum Chem, 2007     

Vieta–Fibonacci wavelets: Application in solving fractional pantograph equations

In this paper, the Vieta–Fibonacci wavelets as a new family of orthonormal wavelets are generated. An operational matrix concerning fractional integration of these wavelets is extracted. A numerical scheme is established based on these wavelets and their fractional integral matrix together with the collocation technique to solve fractional pantograph equations. The presented method reduces solving the problem under study into solving a system of algebraic equations. Several examples are provided to show the accuracy of the method.     

A theoretical prediction for exclusive decaysB→K(K*)η c

The decay rates for the exclusiveB decaysBK _c andBK* _c are calculated in the context of the heavy quark effective theory. We obtain(BK _c )/ (BK)=1.6±0.2 and(BK* _c )/ (K*)=0.39±0.04. These results lead to estimates BR(BK _c )=(0.11±0.02)% and BR(BK* _c )=(0.05±0.01)% if we use the central current experimental values forB(K, K ^*) branching ratios.