Ion pairing, H-bonding, and π–π interactions in copper(II) complex-organo-networks derived from a proton-transfer compound of the 1,10-phenanthroline-2,9-dicarboxylic acid

The one-pot reaction between the novel proton transfer compound (pydaH₂)²⁺(phendc)²⁻, LH₂, and Cu(II) afforded the compounds (pydaH)₂[Cu(phendc)₂]·10H₂O, 1, and (pydaH)₂[Cu(phendc)(phendcH)]₂·5H₂O, 2, where pyda=2,6-diaminopyridine, and phendcH₂=1,10-phenanthroline-2,9-dicarboxylic acid. The single crystal X-ray diffraction analysis of 1 and 2 revealed that these are two novel self-assembled 3D Cu(II) complex-organo-networks, in which (pydaH)⁺ ions and [Cu(phendc)₂]²⁻ or complex units are held together by ion pairing, H-bonding, and π–π interactions. Magnetic measurements over the temperature range 1.8–310 K revealed no significant magnetic coupling between Cu(II) centers in 1 or 2.     

Validated HPTLC and HPLC methods for determination of fluorometholone and sodium cromoglycate in presence of their impurities and degradation products; application to kinetic study and on rabbit aqueous humor

Fluorometholone (FLM) and Sodium Cromoglycate (CMG) are co-formulated in ophthalmic preparation and showed marked instability under different conditions. Two specific, sensitive and precise stability-indicating chromatographic methods have been developed and validated for their determination in the presence of their degradation products and FLM impurity. Ten components were efficiently separated by them. The first method was HPTLC-spectrodensitometry, where the separation was achieved using silica gel 60?F₂₅₄ HPTLC plates and developing system of ethyl acetate: methanol (9:1, v/v). The second method was a reversed phase HPLC associated with kinetic study of the degradation process and was successfully applied for determination of the studied compounds in spiked rabbit aqueous humor. The mobile phase was acetonitrile: methanol: 0.05?M potassium dihydrogenphosphate (0.1% trimethylamine); pH 2.5, adjusted with orthophosphoric acid (20: 30: 50, by volume). In both methods, the separated components were detected at 240?nm and system suitability was checked. Good correlation was obtained in the range of 0.10–24.00 and 0.20–48.00?µg band^?1, for FLM and CMG by HPTLC. While for HPLC, the linearity ranges from 0.01–50.00 and 0.05–50.00?µg?mL^?1 for both drugs. The methods were applied in pharmaceutical formulation, where they were compared to the reported method with no significant difference.     

Attraction behaviour of Anagrus nilaparvatae to remote lemongrass (Cymbopogon distans) oil and its volatile compounds

Utilisation of Anagrus nilaparvatae is a promising and effective method for planthoppers manipulation. Twenty-seven components of remote lemongrass (Cymbopogon distans) oil were identified by GC/MS and nine volatiles were selected for behavioural experiments. In this study, we noted that the remote lemongrass oil was attractive to female A. nilaparvatae at concentrations of 0.1 and 1 mg/L. α-Pinene, β-pinene, eucalyptol, carveol and D-carvone attracted female wasps in the dose-dependent bioassays. Blend 1 (a mixture of eucalyptol, D-carvone, carveol, α-pinene, and β-pinene with ratios of remote lemongrass oil volatiles of 625:80:11:5:3) attracted female wasps at 10 mg/L, while blend 2 (a mixture of the same five volatiles at the same loading ratio) attracted them at 0.1 and 1 mg/L. These results suggested that plant essential oils could be attractants for natural enemies to control pests. The ratios of volatiles in the mixtures affect the attractiveness of the synthetic mixtures.     

Characterization and performance of Pd/Ni(Zn)-aluminate catalysts for acetylene hydrogenation

Research on Chemical Intermediates - 0.03 wt% Pd catalysts on nickel and zinc aluminate supports were prepared by impregnation. The samples were characterized by XRD, BET, ICP, SEM, EDS,...     

An overview on synthetic strategies to coumarins

Coumarins units have recently emerged as a hot topic of research due to their diverse applications. Their synthesis is partly based on classical methodologies such as Pechmann reaction or Knoevenagel condensation, but it also sparked the discovery of completely new pathways. In very recent years so-called vertically expanded coumarins were synthesized, effectively expanding the portfolio of existing architectures. This review serves as a guide through synthesis strategies to coumarins.     

Commercially available 5'-DMT phosphoramidites as reagents for the synthesis of vinylphosphonate-linked oligonucleic acids

[reaction: see text]. Commercially available cyanoethyl phosphoramidites derived from T, d(C), d(A), and d(G) were hydrolyzed (1H-tetrazole, MeCN/H2O) to give the corresponding H-phosphonates in excellent yields. Palladium(0)-catalyzed cross-coupling of each of these with the thymidine-derived vinylbromide 2 afforded the corresponding vinylphosphonate-linked dimers TT, d(C)T, d(A)T, and d(G)T in modest to good yields. The TT dimer was further elaborated to give a 5'-DMT-TT-3'-CEP building block, and this was used in the automated synthesis of the TpTTpT tetramer.     

Synthesis of new water soluble diorganotin(IV) complexes with hydrazones derived from Girard-T reagent as antibacterial and anticancer agents

Three new water-soluble organotin complexes R₂Sn(5-BrSalGT)Cl [R = Ph, Me] and Ph₂Sn(2-OHNaphGT)Cl have been synthesized by the reaction of R₂SnCl₂ (R = Ph or Me) with Schiff bases derived from condensation of Girard-T reagent with 5-bromosalicylaldehyde and 2-naphthaldehyde, (5-BrH₂SalGT)Cl (1) and (2-OHH₂NaphGT)Cl (2). The synthesized compounds have been investigated by elemental analysis, conductometric measurements, IR, ¹H NMR, and ¹¹⁹Sn NMR spectroscopy. These data show that the deporotonated ligand is coordinated to Sn(IV) via ONO atoms and six-coordinate zwitterionic complexes are formed. The ligands and their complexes were investigated for their in vitro toxicity against Gram-positive (Bacillus subtilis and Staphylococcus aureus) and Gram-negative (Escherichia coli and Pseudomonas aeruginosa) bacteria. The results show remarkable antibacterial activity against the studied bacteria. All complexes exhibit more inhibitory effects than the parent ligand. The anticancer activity of all compounds were also performed on HN5 cell line and (2-OHH₂NaphGT)Cl with concentration of 1 mg mL^?1 was found to show higher anticancer activity than other compounds.     

Isolation,characterization, and quantification of curcuminoids and their comparative effects in cerebral ischemia

The study reports a rapid and short analytical technique for separation, characterization, and quantitation along with comparative pharmacological effect of curcuminoids in cerebral ischemia. Flash chromatography, using silica and diol columns along with gradient mobile phase, was utilized to separate three curcuminoids, i.e., curcumin (Cur), demethoxycurcumin (DMC), and bisdemethoxycurcumin (BDMC) for the first time. The separated peaks were monitored at 200–360?nm, whereas the purity of compounds (96.2–97.6%) was determined through qualitative analysis such as infrared and ¹H and ¹³C-nuclear magnetic resonance spectroscopy, mass spectrometry (MS), and differential scanning calorimetry. Furthermore, chitosan nanoparticles (CS-NPs) for curcuminoids were prepared and characterized through zeta sizer, zeta potential, scanning electron microscopy, and transmission electron microscopy. The developed ultra performance of liquid chromatography-electrospray ionization-quadrupole-time of flight-mass spectrometry/mass spectrometry (UPLC-ESI-Q-TOF-MS/MS) method showed simplified automation and shorter run time for Combi flash over conventional separation techniques. The CS-NPs for all the three curcuminoids and combined-curcuminoids (CCr) (combined and administered together for a synergistic effect), following intranasal administration in middle cerebral artery–occluded rats were evaluated for grip strength, locomotor activity, and histopathological examination where the anti-ischemic activity was observed, in terms of potency, for all three CS-NPs and CCr as CCr>Cur>DMC>>BDMC. Cur-CS-NPs exhibited more potency among Cur, DMC, and BDMC, whereas CCr was the more potent anti-ischemic drug compared to Cur, DMC, and BDMC. For Cur the characteristic activity is proposed because of the presence of methoxy group on the phenyl ring whereas for CCr it is synergistic effect of curcuminoids.     

Green synthesis of ZnCo<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles by <Emphasis Type=Italic>Aloe albiflora</Emphasis> extract and its application as catalyst on the thermal decomposition of ammonium perchlorate

This work aimed the evaluation of pH influence in the obtainment of composites from palygorskite (PAL) and chitosan (CS). The materials PAL/CS-1 and PAL/CS-2 were obtained by similar methodology with modified pHs: 5.0 ± 0.5 and 11.0 ± 0.5, respectively. Both materials were evaluated for specific surface area analysis, elemental analysis, XRD, FTIR, thermal analysis, MEV and interaction drug composite, using 5-aminosalicylic acid (5-ASA) as model. The surface area analysis data showed the reduction in PAL/CS-2 related to CS presence on surface in contrast with PAL/CS-1, which corroborate with elemental analysis present nine times more of CS in PAL/CS-2 composition. Regarding to XRD data, the interaction of CS with PAL did not cause modification in clay structure in PAL/CS-2. These results were confirmed by FTIR data with the N–H deformation vibration in PAL/CS-2 while PAL/CS-1 was invariable to PAL. In thermal analysis, results were observed 60.2% residual mass to PAL/CS-2, which it was lower than PAL (87.2%) and PAL/CS-1 (86.7%), due to CS decomposition which had enthalpy energy of 62.1 J g^?1 K^?1, confirming the data previously cited. PAL/CS-2 presented 5-ASA adsorption of 7.9 mg g^?1, which was inferior to others probably caused by scarcity of active sites of PAL already occupied by CS. These results showed that pH control was fundamental to enhance efficiency of obtainment of composite in basic pH because the decrease in CS protonation degree increasing interaction between this one and PAL, although it contributed to decrease in 5-ASA adsorption due to low availability of interaction sites.