2,9-disubstituted 1,10-phenanthroline nickel complexes: Syntheses,characterization, and their ethylene oligomerization

Nickel complexes 1–4 ligated with 2,9-disubstituted-1,10-phenanthroline were synthesized and characterized by FT-IR spectra and elemental analysis. The molecular structure of complex 2 was confirmed by X-ray crystal diffraction analysis. Activated with methylaluminoxane (MAO), those complexes showed moderate activities for ethylene oligomerization. Published in Kinetika i Kataliz, 2007, Vol. 48, No. 5, pp. 710–714. This article was submitted by the authors in English.     

Synthesis of Highly Functionalized Isoxazolinediones from One-pot Reaction of Alkylidene Meldrum ’s Acid with Alkyl Isocyanides in the Presence of Arylhydroxylamines

Alkyl isocyanides undergo a smooth reaction with alkylidene Meldrum’s acids in the presence of arylhydroxylamines to produce N ¹-alkyl-2-(3,5-dioxo-2-aryltetrahydro-4-isoxazolyl)alkanamides in high yields.     

Mechanisms of n‐butanol formation in butyl acrylate latexes

The mechanisms involved in the formation of n‐butanol during the synthesis of butyl acrylate containing latices were investigated. The experimental results showed that neither the hydrolysis of butyl acrylate nor of the ester bond in the butyl acrylate segments of the polymer played a major role in the formation of n‐butanol, which was mainly generated from the polymer backbone, by transfer reactions to polymer chain followed by cyclization. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 5838–5846, 2007     

Self‐assembly of amphiphilic tris(2,2′‐bipyridine)ruthenium‐cored star‐shaped polymers

Amphiphilic tris(2,2′‐bipyridine)ruthenium‐cored star‐shaped polymers consisting of one polystyrene block and two poly(N‐isopropylacrylamide) blocks were prepared by the “arm‐first” method in which RAFT polymerization and nonconvalent ligand–metal complexation were employed. The prepared amphiphilic star‐shaped metallopolymers are able to form micelles in water. The size and distribution of the micelles were studied by dynamic light scattering and transmission electron microscopy techniques. Preliminary studies indicate that the polymer concentration and the hydrophilic poly(N‐isopropylacrylamide) block length can affect the morphologies of the formed metal‐interfaced core–shell micelles in water. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 4204–4210, 2007     

Arsenic determination in marine sediment using ultrasound for sample preparation.

This work deals with As determination in marine sediment using ultrasound for sample preparation. It is shown that As can be quantitatively extracted from marine sediment using 20% (v/v) HCl and sonication. The slurry is centrifuged and the analyte is determined in the supernatant by hydride generation atomic absorption spectrometry (HG AAS). A flow injection (FI) system is employed for hydride generation, with 0.5% (m/v) NaBH(4) used as reducdant and a 20% (v/v) HCl used as sample carrier. The limit of quantification is 1.6 microg g(-1) of As, which is based on 800 microl of sample solution and 0.200 g of sample mass in a volume of 50 mL. Certified and non certified marine sediment samples were analyzed; the results were in accordance with the certified or reference values. Speciation analysis by HPLC-ICP-MS showed that As(V) is the only detectable As species present in the supernatant of the centrifuged sample.     

Selective Propargylation of Carbonyl Compounds and Imines with Barium Reagents

A Barbier‐type regioselective propargylation of aldehydes and ketones with (3‐bromobut‐1‐ynyl)trimethylsilane has been achieved using reactive barium as a low‐valent metal in THF. Especially in the case of ketones, the corresponding homopropargylic alcohols form almost exclusively. In the reaction of α,β‐unsaturated carbonyl compounds, only 1,2‐adducts have been observed. This method is also applicable to propargylation of imines, and the corresponding homopropargylic amines are obtained regiospecifically in good yields with diastereomeric ratios of up to 87:13.     

Synthesis and Characterization of Silica@Copper Core–Shell Nanoparticles: Application for Conjugate Addition Reactions

Silica@copper (SiO₂@Cu) core–shell nanoparticles were synthesized and well characterized by XRD, TEM, AFM, XPS, UV/Vis, TGA–MS, and ICP–AES techniques. The synthesized SiO₂@Cu core–shell nanoparticles were employed as catalysts for the conjugate addition of amines to α,β‐unsaturated compounds in water to obtain β‐amino carbonyl compounds in excellent yields in shorter reaction times. Furthermore, the catalyst works well for hetero‐Michael addition reactions of heteroatom nucleophiles such as thiols to α,β‐unsaturated compounds. As the reaction is performed in water, it allows for easy recycling of the catalyst with consistent activity.     

Efficient method for the direct preparation of aryl carboxylates from carboxylic acids using tosyl chloride under solvent-free conditions

A simple, clean and efficient solvent-free procedure for the preparation of aryl carboxylates is described from the direct reaction of carboxylic acids and phenols, in the presence of 1-methylimidazole as base and tosyl chloride (TsCl) as coupling agent. This method can be easily applied for different substituted phenols and carboxylic acids. It can also be applied for the selective acylation when other functional group such as hydroxyl is present on phenol ring.     

2‐Amino‐4‐chloro‐6‐[N‐methyl‐N‐(4‐methylphenyl)amino]pyrimidine: formation versus fragmentation of hydrogen‐bonded chains of edge‐fused R22(8) rings in 4,6‐disubstituted 2‐aminopyrimidines

Molecules of the title compound, C₁₂H₁₃ClN₄, are linked by two independent N—H...N hydrogen bonds into a chain of edge‐fused R₂²(8) rings. The significance of this study lies in its attempt to rationalize the patterns of supramolecular aggregation in the title compound and in a range of analogous 4,6‐disubstituted 2‐aminopyrimidines.