Inverse colloidal crystal membranes for hydrophobic interaction membrane chromatography

A collaborative study on the robustness and portability of a capillary electrophoresis‐mass spectrometry method for peptide mapping was performed by an international team, consisting of 13 independent laboratories from academia and industry. All participants used the same batch of samples, reagents and coated capillaries to run their assays, whereas they utilized the capillary electrophoresis‐mass spectrometry equipment available in their laboratories. The equipment used varied in model, type and instrument manufacturer. Furthermore, different types of sheath‐flow capillary electrophoresis–mass spectrometry interfaces were used. Migration time, peak height and peak area of ten representative target peptides of trypsin‐digested bovine serum albumin were determined by every laboratory on two consecutive days. The data were critically evaluated to identify outliers and final values for means, repeatability (precision within a laboratory) and reproducibility (precision between laboratories) were established. For relative migration time the repeatability was between 0.05 and 0.18% RSD and the reproducibility between 0.14 and 1.3% RSD. For relative peak area repeatability and reproducibility values obtained were 3–12 and 9–29% RSD, respectively. These results demonstrate that capillary electrophoresis‐mass spectrometry is robust enough to allow a method transfer across multiple laboratories and should promote a more widespread use of peptide mapping and other capillary electrophoresis‐mass spectrometry applications in biopharmaceutical analysis and related fields.     

Synthesis and mesomorphic characterization of azoesters with a coumarin ring

We have synthesized a homologous series of azoesters consisting of a coumaryl moiety as the end group. Eleven derivatives of this series exhibit mesomorphism. The nematic mesophase is exhibited from ethyl homologue onward, while the smectic phase commences at the pentyl derivative and is exhibited along with the nematic phase up to the hexadecyl derivative. The N-I transition temperatures curves show the usual odd-even effect. All the compounds in this series are thermally stable and exhibit a wide mesomorphic range of nearly 120°C. Their thermal stabilities and other characteristics are discussed.     

Nitrenium Salts in Lewis Acid Catalysis

Molecular compounds featuring nitrogen atoms are typically regarded as Lewis bases and are extensively employed as donor ligands in coordination chemistry or as nucleophiles in organic chemistry. By contrast, electrophilic nitrogen‐containing compounds are much rarer. Nitrenium cations are a new family of nitrogen‐based Lewis acids, the reactivity of which remains largely unexplored. In this work, nitrenium ions are explored as catalysts in five organic transformations. These reactions are the first examples of Lewis acid catalysis employing nitrogen as the site of substrate activation. Moreover, these compounds are readily accessed from commercially available reagents and exhibit remarkable stability toward moisture, allowing for benchtop transformations without the need to pretreat solvents.     

Framework Effects on Activation and Functionalisation of Methane in Zinc-Exchanged Zeolites

The first selective oxidation of methane to methanol is reported herein for zinc-exchanged MOR (Zn/MOR). Under identical conditions, Zn/FER and Zn/ZSM-5 both form zinc formate and methanol. Selective methane activation to form [Zn-CH₃]⁺ species was confirmed by ¹³C MAS NMR spectroscopy for all three frameworks. The percentage of active zinc sites, measured through quantitative NMR spectroscopy studies, varied with the zeolite framework and was found to be ZSM-5 (5.7 %), MOR (1.2 %) and FER (0.5 %). For Zn/MOR, two signals were observed in the ¹³C MAS NMR spectrum, resulting from two distinct [Zn-CH₃]⁺ species present in the 12 MR and 8 MR side pockets, as supported by additional NMR experiments. The observed products of oxidation of the [Zn-CH₃]⁺ species are shown to depend on the zeolite framework type and the oxidative conditions used. These results lay the foundation for developing structure–function correlations for methane conversion over zinc-exchanged zeolites.     

Synthesis of 2, 2-Dimethyl-2H-chromenes via a Palladium (II) Catalysed Reaction

The antijuvenile hormones Precocene-I, Precocene-II and other bioactive 2, 2-dimethyl-2H-chromenes have been synthesised by intramolecular oxidative cyclisation of 2-isoprenyl phenols catalysed by a palla-dium(II) salt.     

Regioselective N‐alkylation for the synthesis of novel aminotriazolophanes

Regioselective synthesis of macrocycles, incorporating 3‐oxo‐4‐amino‐1,2,4‐triazole derivatives, has been achieved by reactions involving N‐alkylation, utilizing appropriate 1, ω ‐dihaloalkanes in the presence of metal hydroxide. © 2006 Wiley Periodicals, Inc. Heteroatom Chem 17:329–336, 2006; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20211     

Phytochemical and antioxidant properties of some Cassia species

In this study, the antioxidant activity of aqueous and ethanol extracts of four plants from the genus Cassia were evaluated by various antioxidant assays, including ferric reducing antioxidant power (FRAP), DPPH free radical scavenging, metal chelating activity, phosphomolybdenum reducing power, hydrogen peroxide radical scavenging, hydroxyl radical scavenging, deoxyribose degradation and β-carotene bleaching assay. The various antioxidant activities were compared to standard antioxidant such as ascorbic acid. All the extracts showed antioxidant activity in the tested methods. Among the four species, Cassia auriculata has been found to possess highest activity in most of the tested models. In addition to the antioxidant activity, the total phenolics and flavonoids were measured in the extracts. The ethanolic extract exhibited highest phenolics and flavonoid contents and had also shown potent antioxidant activity in comparison to the aqueous extracts. The possible antioxidant mechanism of the ethanol extract can be due to its hydrogen or electron donating and direct free radical scavenging properties. Hence, the ethanol extract represents a source of potential antioxidants that could be used in pharmaceutical industries.     

Cyanoethylation of methyl and ethyl ethers of dimethylphenols

The C-cyanoethylation of the methyl and ethyl ethers of dimethylphenols has been carried out with acrylonitrile in the presence of anhydrous AlCl₃ to furnish propionitrile derivatives. The latter on hydrolysis to the corresponding propionic acids followed by cyclization with PPA afforded the appropriate indanones, whose structures have been established on the basis of spectral data and by the formation of 2, 4-DNP derivatives.     

Band gap determination in lead iodide polytypes

The band gaps of the polytypic crystals of lead iodide have been determined by studying the temperature variation of conductivity. Results obtained on several polytypic crystals show that the band gaps of the higher polytypes are lower than that of the parent 2H structure (2.56 eV). As for example the band gaps for 12H, 14H, 18H and 20H (disordered) were found to be 1.65, 1.44, 1.07 and 1.01 eV. The significance of the band gap determination in regard to the recent anomalous results on the physical properties of lead iodide crystals, has been indicated.