CuSO<Subscript>4</Subscript> as a Mild,Green, and Efficient Catalyst for the One-pot Conversion of <Emphasis Type="Italic">THP</Emphasis> Ethers to Acetates

Summary. An efficient direct conversion of THP ethers into the corresponding acetates was achieved with acetic anhydride in the presence of CuSO₄ · 5H₂O as an available and green catalyst in high yields.     

Stereospecific synthesis of 1,2-cis glycosides by vinyl-mediated IAD

[reaction: see text] Stereospecific 1,2-cis glycosylation of 2-O-vinyl thioglycosides, synthesized from the corresponding alcohols by Ir-catalyzed transvinylation with vinyl acetate, is achieved by iodine-mediated tethering of a range of primary and secondary carbohydrate acceptors, followed by intramolecular aglycon delivery (IAD). The use of such an intramolecular glycosylation strategy furnishes the desired alpha-gluco and beta-manno disaccharides in an entirely stereoselective manner.     

Fe(Cp)2PF6: An efficient catalyst for cyanosilylation of carbonyl compounds under solvent free condition

An efficient method for the addition of trimethylsilyl cyanide (TMSCN) to various aldehydes and ketones has been described using Fe(Cp)₂PF₆ (2.5 mol%) as a catalyst under solvent free condition. Excellent yields of trimethylsilylether of cyanohydrin up to (94%) was achieved within 10 min.     

Headspace solvent microextraction A new method applied to the preconcentration of 2-butoxyethanol from aqueous solutions into a single microdrop

A new procedure and experimental setup for the headspace solvent microextraction of volatile organic materials from aqueous sample solutions is described. The extraction occurs by suspending a 3-μl drop of the solvent from the tip of a microsyringe to the headspace of a stirred aqueous sample solution for a preset extraction time. The temperature of the microdrop and the bulk of sample solution should be kept constant at optimized values. The sample analyses were carried out by gas chromatography. The procedure was successfully applied to the extraction and determination of 2-butoxyethanol from content of some color samples used for painting the outer coverage of some machines such as coolers, refrigerator, cloths machine, etc. Parameters such as extraction time, nature of extraction solvent, size of microdrop, sample volume, stirring rate, ionic strength and pH of sample solution were studied and optimized, and the method performance was evaluated.     

Etude du Systeme Ternaire Se-Te-Sn

This work is a part of the systematic study of the ternary based chalcogenides systems. The aim is to determine the phase equilibrium, and to determine the limits of the phase area. This is done in view to perfecting knowledge of elaboration conditions for new materials and to study of their physical properties. Few works have been devoted to the study of the ternary system Se-Te-Sn, only the cross section SnSe-SnTe has been studied [1] and [2]. The experimental study by DTA, DSC and X-ray diffraction on powder performed at room temperature, exhibits a miscibility gap in the liquid state which narrows as it goes through the Sn-Se binary system. Three cross sections behave as ‘quasi-binary‘ system and six ternary invariants have been exhibited: three ternary eutectics and three ternary quasi-peritectics. This revised version was published online in July 2006 with corrections to the Cover Date.     

Novel coated-graphite membrane sensor based on N,N′-dimethylcyanodiaza-18-crown-6 for the determination of ultra-trace amounts of lead

A novel selective membrane electrode for determination of ultra-trace amount of lead was prepared. The PVC membrane containing N,N′-dimethylcyanodiaza-18-cown-6 (DMCDA18C6) directly coated on a graphite electrode, exhibits a Nernstian response for Pb²⁺ ions over a very wide concentration range (from 1.0×10⁻² to 1.0×10⁻⁷ M) with a limit of detection of 7.0×10⁻⁸ M (∼14.5 ppb). It has a fast response time of ∼10 s and can be used for at least 2 months without any major deviation in potential. The electrode revealed very good selectivity with respect to all common alkali, alkaline earth, transition and heavy metal ions. The proposed sensor was used as an indicator electrode in potentiometric titration of lead ions and in determination of lead in edible oil, human hair and water samples. The proposed sensor was found to be superior to the best Pb²⁺-selective electrodes reported in terms of detection limit and selectivity coefficient.     

Catalytic Method for Synthesis of Aspirin by a Green,Efficient and Recyclable Solid Acid Catalyst (Preyssler's Anion) at Room Temperature

Synthesis of aspirin at room temperature via O‐acetylation of salicylic acid in the presence of Preyssler type heteropolyacids has been investigated in order to contribute toward clean technology, which is the most important need of the society. All of the catalysts are recyclable and reusable.     

The synthesis of unsymmetrically N-substituted chiral 1,4,7-triazacyclononanes

A number of chiral unsymmetrically N-substituted 1,4,7-triazacyclononane ligands have been prepared by modular methods. The key step in the synthesis centres on the macrocyclisation of three tertiary amide precursors under standard Richman-Atkins conditions which allows for subsequent N-functionalisation.     

Synthesis,Characterization and Crystal Structures of new Palladium(II) Complexes and the first Platinum(III) Complex Containing ATT (ATT = 6‐Aza‐2‐thiothymine)

Treatment of the ligand 6‐aza‐2‐thiothymine (ATT, HL, 1 ) with palladium chloride in methanol forms the ionic complex [(HL)₄Pd]Cl₂·8MeOH ( 2 ), while its reaction with palladium iodide in same solvent produces the neutral complex trans‐[(HL)₂PdI₂]·2MeOH ( 3 ) in high yields. The reaction of 1 with Na₂[PdCl₄] in the presence of sodium acetate in a molar ratio of 2:1:2 and with platinum(II) chloride in presence of sodium acetate led to the dimer tetranuclear complexes [(L₄Pd₂)NaCl]₂·8MeOH ( 4 ) and [L₄Pt₂Cl₂]·6MeOH·H₂O ( 5 ). The latter is the first Pt^III complex of the ligand. All complexes were characterized by elemental analyses and IR spectroscopy and the crystal structures of 2 , 3 , 4 and 5 are determined by single‐crystal X‐ray diffraction. Crystal data for 2 at ?80 °C: triclinic space group , a = 1006.6(1), b = 1006.9(1), c = 1158.1(1) pm, α = 85.20(1)°, β = 83.84(1)°, γ = 88.91(1)°, Z = 1, R₁ = 0.0278; for 3 at ?80 °C: triclinic space group , a = 490.5(1), b = 977.2(2), c = 1116.8(2) pm, α = 90.26(1)°, β = 102.33(1)°, γ = 96.08(1)°, Z = 1, R₁ = 0.0394; for 4 at ?80 °C: orthorhombic space group Ccca, a = 1791.7(2), b = 1874.1(2), c = 2044.0(1) pm, Z = 4, R₁ = 0.0341 and for 5 at ?80 °C: monoclinic space group P2₁/c, a = 1464.3(1), b = 2003.7(1), c = 1368.5(1) pm, β = 95.66(1)°, Z = 4, R₁ = 0.0429.     

Pyrazine Complexes of Octacyanometallates of Mo(IV) and W(IV) With 8-hydroxyquinoline: Synthesis,characterisation and thermal studies

The complexes formed by photosubstitution of pyrazine (Pz) in octacyanomolybdate(IV) and -tungstate(IV) with 8-hydroxyquinoline have been assigned the formulae [Mo(CN)₂(OH)₂(Pz)₂(OX)] and [W(CN)₂(OH)₂(Pz)₂(OX)·1.5H₂O]. Coordination of Pz as an unidentate ligand by donating a lone pair of electron from nitrogen is shown by an absorption peak between 8–11 µ. Mechanism for the thermal decomposition of the complexes has been given. The formation of tungsten metal as residue in case of II has been confirmed by XRD analysis. The kinetic and thermodynamic parameters like activation energy (E _a), pre-exponential factor (A) and entropy of activation (S ^#) were calculated employing different integral methods of Doyle, Coats and Redfern and Arrhenius.H for each stage of decomposition was obtained from DSC.This revised version was published online in November 2005 with corrections to the Cover Date.