Infrared spectroscopy is used to investigate the transformation of carboxyl-terminated alkyl chains immobilized on a surface into succinimidyl ester-terminated chains by reaction with an aqueous solution of N-ethyl-N'-(3-(dimethylamino)propyl)carbodiimide (EDC) and N-hydroxysuccinimide (NHS). The acid chains are covalently grafted at the surface of hydrogenated porous silicon whose large specific surface area allows for assessing the activation yield in a semiquantitative way by infrared (IR) spectroscopy and detecting trace amounts of surface products and/or reaction products of small IR cross section. In this way, we rationalize the different reaction paths and optimize the reaction conditions to obtain as pure as possible succinimidyl ester-terminated surfaces. A diagram mapping the surface composition after activation was constructed by systematically varying the solution composition. Results are accounted for by NHS surface adsorption and a kinetic competition between the various EDC-induced surface reactions.
The synthesis and characterisation by elemental analysis, conductivity, FTIR, UV-Visible, ESR and magnetic measurements are described for a series of complexes of nickel(II) and cobalt(II) with three ligands (H 2 L 1-3 ) derived from reduced N, N 0 -o-Phenylenebis(salicylideneimine). The complexes formed are identified as neutral species, where the ligands are coordinated through N and O donor atoms. The formulae obtained for the complexes are: [CoL(H 2 O) 2 ] with octahedral geometry and [NiL] with tetrahedral geometry. Their antifungal activity is evaluated towards human pathogenic fungi including yeasts of the Candida genus, some opportunistic moulds belonging to the Aspergillus, Scedosporium genus and some dermatophytes. The cobalt complexes show a significant growth inhibition of yeasts tested and also to fungi of the genus Scedosporium which is of interest because these fungi are usually poorly susceptible to current antifungal including Amphotericin B and Itraconazole, chosen as reference in this study. The activity data show that the metal complexes are more potent than the parent ligand.
Bi-or polydentate ligands based on heterocycles can be easily prepared by palladium-catalysed C-H bond activation of heteroaromatics followed by heteroarylation with heteroaryl bromides. A variety of heteroaromatics such as furans, thiophenes, pyridines, thiazoles or oxazole derivatives have been employed and moderate to good yields were generally ob-
The palladium-catalyzed direct 2- or 5-arylation of some free NH(2)-substituted thiophene derivatives was found to proceed in high yields using a variety of aryl bromides. In the course of these reactions, no coupling of the aryl bromide with the thiophene NH(2) substituent was detected. The presence of an ester substituent on C2 of thiophene was found to be useful to block this highly reactive carbon.
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