Silver-catalyzed cycloisomerization of 1,n-allenynamides

A variety of allenynamides can undergo cycloisomerization reactions in the presence of silver triflate thus leading to the formation of N-containing heterocycles incorporating cross-conjugated trienes. Access to new dienic 4-piperidinone and azepane motifs was achieved. An extension to one-pot tandem sequences involving silver-catalyzed cycloisomerization/Diels-Alder reaction was also examined.     

SYNTHESIS AND SOME REACTIONS OF 2-MERCAPTO-3,5,7-TRIPHENYLPYRIDO[2,3-d]-PYRIMIDINE-4(3H)-ONE

Abstract

2-Mercapto-3,5,7-triphenylpyrido[2,3-d]pyrimidine-4(3H)-one (II) was synthesized by the interaction of ethyl-2-amino-4,6-diphenylincotinate (I) with phenyl isothiocyanate in pyridine. The reaction of II with different reagents was carried out to give some condensed heterocyclic systems.     

A comparative study of energy consumption and physical properties of microfibrillated cellulose produced by different processing methods

Microfibrillated celluloses (MFCs) with diameters predominantly in the range of 10–100 nm liberated from larger plant-based fibers have garnered much attention for the use in composites, coatings, and films due to large specific surface areas, renewability, and unique mechanical properties. Energy consumption during production is an important aspect in the determination of the “green” nature of these MFC-based materials. Bleached and unbleached hardwood pulp samples were processed by homogenization, microfluidization, and micro-grinding, to determine the effect of processing on microfibril and film properties, relative to energy consumption. Processing with these different methods affected the specific surface area of the MFCs, and the film characteristics such as opacity, roughness, density, water interaction properties, and tensile properties. Apparent film densities were approximately 900 kg/m³ for all samples and the specific surface area of the processed materials ranged from approximately 30 to 70 m²/g for bleached hardwood and 50 to 110 m²/g for unbleached hardwood. The microfluidizer resulted in films with higher tensile indices than both micro-grinding and homogenization (148 Nm/g vs. 105 Nm/g and 109 Nm/g, respectively for unbleached hardwood). Microfluidization and micro-grinding resulted in films with higher toughness values than homogenization and required less energy to obtain these properties, offering promise for producing MFC materials with lower energy input. It was also determined that a refining pretreatment required for microfluidization or homogenization can be reduced or eliminated when producing MFCs with the micro-grinder. A summary of the fiber and mechanical energy costs for different fibers and processing conditions with economic potential is presented.     

Synthesis of pyrazolo[4,3-d]oxazoles

1-Phenyl-3-methyl-5-pyrazolone-4-oxime reacted with benzylamine, methylamine, methyl- and ethyl ioides to give 3-methyl-1,5-diphenyl-1H-, 3-methyl-1-phenyl-1H- and 3,5-dimethyl-1-phenyl-1H-pyrazolo[4,3-d]oxazoles I, II. The structure of I was elucidated authentically through other routes by interaction of 1-phenyl-3-methyl-4,5-dioxopyrazolone with benzylamine and/or benzaldehyde and ammonium acetate. Various 3-meth-yl-5-aryl-1-phenyl-1H-pyrazolo[4,3-d]oxazoles IV were synthesized by the reaction of 4,5-dioxopyrazolone with aromatic aldehydes in the presence of ammonium acetate. Also, the structure of I was elucidated authentically via other routes by the reaction of 1-phenyl-3-methyl-4-imino-5-pyrazolone with each of benzylcyanide, benzylamine, benzaldehyde and benzalaniline.     

Spectrophotometric and derivative spectrophotometric study of the reaction of palladium (II) and rhodium (III) with 5-(3,4-methoxyhydroxybenzylidene)rhodanine and cationic surfactants

Spectrophotometric and derivative spectrophotometric methods for the determination of Pd(II) and Rh(III) are proposed. Pd(II) forms with 5-(3,4-methoxyhydroxybenzylidene)rhodanine [3,4-MHBR], in the absence and presence of cetylpyridinium bromide [CPB], 14 binary and 134 ternary complexes having molar absorptivities of 5.77 × 10⁴ and 7.46 × 10⁴ M ^–1cm^–1 at 525 and 530 nm, respectively. Rh(III) forms a 14 complex with 3,4-MHBR in the presence of cetyltrimethylammonium bromide [CTAB], which gives a maximum absorbance at 445 nm with a molar absorptivity of 5.13 × 10⁴ M ^–1cm^–1. Derivative spectrophotometric methods are employed for the determination of Pd(II) and Rh(III) at ng ml^–1 levels utilizing these complexes. Under the optimum conditions the calibration lines for Pd(II) and Rh(III) determination fit the equations d⁴ A/d⁴ = 1.10 × 10⁶ [Pd] – 0.018 (r = 0.9967) and d⁴ A/d⁴ = 2.25 × 10⁶ [Rh] + 0.03 (r = 1.0426) and have detection limits of 5.6 and 1.2 ng ml^–1, respectively. The influences of experimental variables and foreign ions are studied. The methods are free of interference from most common metal ions and anions. The results of the analysis of some synthetic mixtures of Pd(II) and Rh(III) are reported.     

Chemical composition and antibacterial activity of the essential oil of Moroccan Juniperus phoenicea

The antibacterial activity of the essential oil from leaves of Juniperus phoenicea (Cupressaceae) and its chemical constituents were investigated in this study. The essential oil was obtained by hydro-distillation and analyzed by gas chromatography equipped with a flame ionisation detector (GC-FID), and gas chromatography coupled to a mass spectrometer (GC-MS). Sixty-three volatile compounds were identified representing 52 to 92% of the total oil compositions. The main monoterpenes were a-pinene (26.7-78.7%) and 6-3carene (7.6-15.4%). The antibacterial activity of J. phoenicea essential oil, when tested against both Gram-positive and Gram-negative bacteria, showed high activity against all bacteria tested, except Pseudomonas.     

On Bounded Solutions for Nonlinear Parabolic Equations with Degenerate Coercivity

Mediterranean Journal of Mathematics - By means of Stampacchia’s lemma, we prove an existence result of bounded solutions for some nonlinear parabolic equations with degenerate coercivity.     

Characterization of Egyptian bronze archaeological artifacts

This paper presents the results of in situ non‐destructive X‐ray fluorescence determination of the chemical analysis of a collection of ten bronze statues that are on display at the Egyptian museum of Cairo. The statues are from the late period of the ancient Egyptian history. In addition, destructive technique X‐ray diffraction analysis was applied on 11 damaged archaeological objects to determine the corrosion products and the alloy compositions. Specimens of the latter objects were subjected to metallographic examinations to determine the microstructure of the alloy. Surprisingly, the results indicated that all ten statues and 10 of the 11 damaged objects were made of lead – bronze alloy; the percentage of the lead varied from 3.43 to 18.04, the tin varied from 2.53 to 10.67. The chemical composition of the patina on eight damaged objects is essentially composed of (Cu₂O) cuprite for all objects in addition to other compounds such as (SnO₂) cassiterite in two objects, (PbCO₃) cerussite in three other objects and (Cu₂(OH)₃Cl) atacamite or (Cu(OH)₃Cl) paratacamite in two other objects. The formation of chlorides and carbonate resulted from the interaction between surrounding environment and the alloy. The results of the metallographic examinations indicated a non‐homogenous structure and the increase of the lead content increases the globular lead particles. In spite of this condition, the galvanic corrosion tendency when the alloy is exposed to moist air or soil is not possible as lead compounds are electrically insulating. Another advantage for using leaded bronze in making statues is being heavy and thus leads to stability. Copyright © 2012 John Wiley & Sons, Ltd.