Intramolecularly coordinated organoantimony(III) carboxylates

The reactions of organoantimony chlorides L^1,2SbCl₂1 and 2 ([2,6-(ROCH₂)₂C₆H₃]⁻, R = Me; L¹ and R = t-Bu; L²) with silver salts of selected carboxylic acids resulted to corresponding organoantimony carboxylates L^1,2Sb(OOCR′)₂, 1a-c (for L¹) and 2a-c (for L²), where R′ = CH₃ for 1a, 2a; R′ = CHCH₂ for 1b, 2b and R′ = CF₃ for 1c, 2c. All compounds were characterized by the help of elemental analysis, ESI-MS, ¹H and ¹³C NMR spectroscopy. The solid state structure investigation using single crystal X-ray diffraction techniques (2a, c) and IR spectroscopy revealed significant differences in coordination mode of both O,C,O chelating ligand and carboxylic groups in this set of compounds. The structure of all compounds in solution of non-coordinating solvent (CDCl₃) was determined by means of variable temperature ¹H, ¹³C, ¹⁹F NMR spectroscopy and IR spectroscopy.     

Self‐Assembly of 1,1′‐Biphenyl‐2,2′,6,6′‐tetracarboxylic Acid: Formation of an Achiral Grid with Chiral Compartments

D ₄ ‐symmetric chiral hydrogen‐bonded cyclotetramers (see the structure in the picture) are present in the self‐assembled achiral title compound in the solid state. The unilayered network set up from the chiral “square” blocks is achiral as a consequence of the crystal symmetry.     

Study of carbon black obtained by pyrolysis of waste scrap tyres

Waste scrap tyres were thermally decomposed under various conditions. Decompositions were followed by the TGA method. Specific heating regimes were tested to obtain optimal structural properties of resulting pyrolytic carbon black produced by pyrolysis of scrap tyres and the process was characterized in temperature interval from 380 to 1,200 °C and heating rate 10, 20 and 50 °C min^?1 under nitrogen atmosphere. The original scrap tyres and pyrolytic carbon black were characterized by Raman and Fourier transform infrared spectroscopy methods. Textural properties were also determined. Effect of temperature and heating rate on process of pyrolysis of scrap tyres was observed. Shifting of temperature of maximum pyrolysis rate to lower value and spreading of DTG peak is caused by increasing heating rate. Temperature 570 °C was sufficient for total scrap tyres pyrolysis. Graphitic and disordered structure was distinguished in the formed carbon black by Raman spectroscopy. With increasing temperature, heating rate and weight loss, the amount of the graphitic structure was reduced at the expense of disordered structure. Destruction of nonporous scrap tyres and formation of porous structure took place at higher temperature. Porous carbon black is formed above 380 °C, specific surface area increased up to 88 m² g^?1 .     

Preparation of planar‐chiral multidonor phosphanylferrocene carboxamides and their application as ligands for palladium‐catalysed asymmetric allylic alkylation

Amide coupling of (S_p)‐2‐(diphenylphosphanyl)ferrocene‐1‐carboxylic acid with appropriate terminal amines mediated by 1‐hydroxybenzotriazole and a carbodiimide affords multi‐donor amides terminally functionalized with planar‐chiral (S_p)‐2‐(diphenylphosphanyl)ferrocen‐1‐yl moieties in good to excellent yields. Palladium catalysts based on these ligands efficiently promote asymmetric allylic alkylation of 1,3‐diphenylallyl acetate with in situ generated dimethyl malonate anion to give the C‐alkylated product with ees up to 93% at room temperature. Copyright © 2010 John Wiley & Sons, Ltd.     

Studies of the forced hydrolysis degradation of copper complexes with different oligosaccharides

Bioactive copper complexes with oligosaccharides, pullulan or dextran, are the objective of the present study, because of their possible biomedical applications. The alkaline and acid hydrolysis of the Cu(II) complexes with reduced low-molar pullulan or dextran were carried out by conductometric method. The influence of ligand constitutions on the stability of the complexes was examined on the basis of ligand property. The complexes degradation during alkaline and acid hydrolysis were carried out in sodium hydroxide and hydrochloric acid solutions of 0.1, 0.5, and 1.0 mol dm⁻³, at different temperature (25, 40, and 60°C, respectively). According to the obtained results by the conductivity investigation during forced degradation studies, it could be concluded that the Cu(II) complexes show the small pharmaceutical stability to both hydrolysis.     

Structure and in vitro antifungal activity of [2,6‐bis(dimethylaminomethyl)phenyl]diphenyltin(IV) compounds

A set of seven [2,6‐bis(dimethylaminomethyl)phenyl]diphenyltin(IV) ({[(CH₃)₂NCH₂]₂(C₆H₃)}­(C₆H₅)₂Sn⁺X^?) ionic organotin(IV) compounds (X = Br, NO₃, CN, SCN, SeCN, BF₄ and PF₆) has been prepared and characterized by electrospray ionization mass spectrometry, ¹H NMR spectroscopy in CDCl₃,¹¹⁹Sn NMR in CDCl₃ and DMSO‐d₆ solution, as well as by ¹³C and ¹¹⁹Sn CP/MAS NMR spectroscopy and X‐ray diffraction techniques in the solid state. The in vitro antifungal activity of these water‐soluble ionic organotin(IV) compounds was compared with starting compounds and the antifungal drugs currently in clinical use. Copyright © 2002 John Wiley & Sons, Ltd.     

Ultrasonic extraction of oil from tobacco (Nicotiana tabacum L.) seeds

The ultrasonic extraction (UE) of oil from the seeds of a semi-oriental tobacco (Nicotiana tabacum L.) plant strain by using n-hexane and petroleum ether was studied at different temperatures and seeds-to-solvent ratios. The oil yield depended on the seed comminution, the extraction temperature, the seeds-to-solvent ratio and the type of solvent. The oil yield was much higher if the seeds were ground before extraction. The oil yield increased with increasing the extraction temperature and with decreasing the seeds-to-solvent ratio. n-Hexane was somewhat more efficient in the oil extraction than petroleum ether. In recovering the tobacco seed oil (TSO), the UE was less efficient than the Soxhlet extraction. The advantage of the UE was a relatively high oil yield at 25 degrees C in a shorter time. The kinetics of UE of TSO was described using the model of unsteady diffusion through plant material.