Efficient and rapid synthesis of polyureas and polythioureas from the reaction of urea and thiourea with diamines under microwave irradiation

Polyureas and polythioureas were readily synthesized by the reaction of aromatic and aliphatic amines with urea and thioureas, respectively, in good to excellent yields under microwave irradiation. The effects of the microwave irradiation time and power, the nature of the solvent, and the solid content of the monomers on the inherent viscosity of the polymers were investigated. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 2106–2111, 2004     

A Straightforward Approach for the Synthesis of Novel Derivatives of Benzo[b]pyrazolo[5′,1′:2,3]pyrimido[4,5‐e][1,4]thiazine

Several derivatives of the novel benzo[b]pyrazolo[5′,1′:2,3]pyrimido[4,5‐e][1,4]thiazine ring system have been synthesized through the one‐pot cyclocondensation of 6‐bromo‐7‐chloro‐2‐(ethylthio)‐5‐methylpyrazolo[1,5‐a]pyrimidine‐3‐carbonitrile ( 4 ) with o‐aminothiophenol in the presence of Et₃N in CH₃CN. The true regio isomer ( 5 ) was also determined by X‐ray crystallographic analysis. The N‐alkylation of the synthesized compound ( 5 ) was also accomplished.     

Preparation of new membranes based on sulfonated aromatic copolyimides

New sulfonated aromatic copolyimides with controlled degree of sulfonation were prepared via polycondensation reactions of a sulfonated diamine and two unsulfonated diamines with 1,4,5,8‐naphthalene tetracarboxylic dianhydride (NDA). The sulfonated diamine 3,3′‐disulfonic acid‐ bis[4‐(5‐amino‐1‐naphthoxy)phenyl]sulfone (DANPS) was synthesized through nucleophilic substitution reaction of 5‐amino‐1‐naphthol with disodium‐3,3′‐disulfonate‐4,4′‐dichlorodiphenysulfone (SDCDPS) and subsequent acidification. Two unsulfonated diamines 4,4′‐(5‐amino‐1‐naphthoxy)diphenylsulfone (ANDS) and 4,4′‐(4‐aminophenoxy)diphenylsulfone (APDS) were prepared by nucleophilic reaction of 5‐amino‐1‐naphthol and 4‐aminophenol with 4,4′‐dichlorodiphenylsulfone in the presence of potassium carbonate, respectively. After characterization of the monomers and polymers with common methods, the physical properties of the polymers including thermal behavior and stability, viscosity, molecular weight, and ion exchange capacity (IEC) were studied. The polymers showed high thermal stability and ion exchange capacity which were the basic requirements for application as fuel cell membranes. Copyright © 2008 John Wiley & Sons, Ltd.     

Simple efficient algorithm (SEA) for shallow flows with shock wave on dry and irregular beds

An explicit Godunov‐type solution algorithm called SEA (simple efficient algorithm) has been introduced for the shallow water equations. The algorithm is based on finite volume conservative discretisation method. It can deal with wet/dry and irregular beds. Second‐order accuracy, in both time and space, is achieved using prediction and correction steps. A very simple and efficient flux limiting technique is used to equip the algorithm with total variation dimensioning property for shock capturing purposes. In order to make sure about the balance between the flux gradient and the bed slope, treatment of the source term has been done using a new procedure inspired mainly by the physical rather than mathematical consideration. SEA has been applied to one‐dimensional problems, although it can equally be applied to multi‐dimensional problems. In order to assess the capability of proposed algorithm in dealing with practical applications, several test cases have been examined. Copyright © 2007 John Wiley & Sons, Ltd.     

Silver Nanoparticles–Polyaniline Nanocomposite for Microextraction in Packed Syringe

A rapid, convenient and reliable method for microextraction in packed syringe (MEPS) of the loop diuretic furosemide (FUR) in urine along with high-performance liquid chromatography (HPLC) was developed. A nanocomposite based on silver nanoparticles/polyaniline (Ag-NPs/PANI) was synthesized and used as the MEPS packing material. This nanocomposite was prepared conveniently using interfacial polymerization without the need for any templates or functional dopants. The feasibility of the synthesized nanocomposites was examined by isolation of FUR from diluted urine samples. After extraction, the analyte was desorbed by 200 μL of methanol. It was then dried and the residue was dissolved in 30 μL of methanol and an aliquot of 25 μL was, finally, injected into the HPLC system. Important parameters influencing the extraction and desorption processes were optimized and 25 cycles of draw–eject gave maximum peak area, when desorption was performed. The linearity was studied by preconcentration of 5 mL of diluted urine sample spiked with a standard solution of FUR in the concentration range of 15–750 μg L^?1. The coefficient of determination was satisfactory (r ² > 0.99) and the relative standard deviation (RSD %) value under the optimized condition was 8.8 %. The limit of detection and limit of quantification were 7 and 15 μg L^?1, respectively.     

Polycondensation of pyridine-2,6-dicarboxylic acid with some di- and tetraamino compounds

Pyridine-2,6-dicarboxylic acid phenyl ester was condensed with 3,3′-diaminobenzidine and 3,3′,4,4′-tetraaminodiphenyl ether. Polyamides were also synthesized by condensation of the above ester with p-phenylenediamine, benzidine, 4,4′-diaminodiphenyl sulfide and 4,4′-diaminodiphenyl sulfone. These amides had higher inherent viscosities and greater thermal stability than was reported before. Model compounds of imidazoles were prepared by condensation of the same ester with o-phenylenediamine and 2,3-diaminopyridine and of polyamides by condensation with aniline and 2-aminopyridine. In the case of the polyimidazole, the completely closed ring of imidazole did not form. The ultraviolet spectra of model compounds were compared with those of the polymers. The thermogravimetric curves show that the polymers are stable up to more than 400°C under argon atmosphere. All polymers were insoluble in most organic and inorganic solvents. They dissolved only partially in DMSO and DMF. Inherent viscosity was measured for the soluble polymer fraction.     

Reconstructing unknown nonlinear boundary conditions in a time‐fractional inverse reaction–diffusion–convection problem

This paper has focused on unknown functions identification in nonlinear boundary conditions of an inverse problem of a time‐fractional reaction–diffusion–convection equation. This inverse problem is generally ill‐posed in the sense of stability, that is, the solution of problem does not depend continuously on the input data. Thus, a combination of the mollification regularization method with Gauss kernel and a finite difference marching scheme will be introduced to solve this problem. The generalized cross‐validation choice rule is applied to find a suitable regularization parameter. The stability and convergence of the numerical method are investigated. Finally, two numerical examples are provided to test the effectiveness and validity of the proposed approach.     

Self-condensation reaction of aromatic tetraamines in polyphosphoric acid

Ladder and partial ladder polymers have been obtained by self-condensation reactions of 1,2,4,5-tetraaminobenzene, 3,3′,4,4′-tetraaminodiphenyl ether, 3,3′-diaminobenzidine and 3,3′,4,4′-tetraaminodiphenyl sulfone in polyphosphoric acid. The products thus obtained are highly colored compounds with good thermal stability. They seem to be made up of polyquinoxaline or dihydrophenazine or a mixture of these two recurring units. They are slightly soluble in methanesulfonic acid and concentrated sulfuric acid and have inherent viscosities in the 0.2 to 0.4 range.     

Polymers containing anthraquinone units: Polycondensations 1,2,5,6-tetraaminoanthraquinone with some tetrachloroquinoxaline compounds

New ladder and partial ladder aromatic heteropolymers have been synthesized from 1,2,5,6-tetraaminoanthraquinone, 2,3,7,8-tetrachloro-1,4,6,9-tetraazaanthracene, 2,2′-3,3′-tetrachloro-6,6′-diquinoxaline, 2,2′,3,3′-tetracholoro-6,6′-diquinoxalyl ether and 2,2′,3,3′-tetrachloro-6,6′-diquinoxalyl sulfone. The polycondensations were carried out in solution and in melt. The inherent viscosities of polymers were in the range of 0.1-0.44. These polymers were highly colored, showed good thermal stability and were soluble in concentrated sulfuric acid and methanesulfonic acid. The structures of the polymers were established by comparison with model compounds.