Efficient (bromodimethyl)sulfonium bromide mediated synthesis of benzimidazoles

Benzimidazoles have been efficiently synthesized in high yields by treatment of 1,2-phenylenediamine with aldehydes using (bromodimethyl)sulfonium bromide at room temperature.     

Measurement of thermal conductivity of fluids using 3-<Emphasis Type="Italic">ω</Emphasis> method in a suspended micro wire

A thermally controlled, compact device employing the 3-ω technique, used to measure the thermal conductivity of fluids, is designed, developed, and presented in this paper. The 3-ω method, which analyzes temperature oscillations data in the frequency domain, requires a microscopic sample and extremely low heating power. The functionality is derived from the approximate solutions of temperature oscillations of a line heater based on the infinite line-heater model over an empirically and analytically chosen range of frequencies. The method is devoid of errors related to transient measurements, fluid thermal stratification and mobility errors, which pose difficulties in other methods. A platinum (99.99% pure) wire of 50 μm diameter and a length of 30 mm, suspended in a sample volume of 25 μl of the test fluid, serves simultaneously as the heater and thermometer. Structure-wise, the device is designed to support measurements over a range of temperatures and fluid pressures providing modularity and flexibility to the instrument. The device is successfully employed to measure the thermal conductivity of de-ionized water for temperatures between 15 and 35°C with an accuracy of ±1.2% inmeasurement.     

A highly chemoselective Boc protection of amines using sulfonic-acid-functionalized silica as an efficient heterogeneous recyclable catalyst

A facile and versatile method for the chemoselective Boc protection of amines has been developed by a treatment with (Boc)₂O in the presence of sulfonic-acid-functionalized silica as a catalyst. The method is general for the preparation of N-Boc derivatives of aliphatic (acyclic and cyclic), aromatic, and heteroaromatic amines; primary and secondary amines; aminols, amino-esters; and sulfonamides. The catalyst works under heterogeneous conditions and can be recycled.     

Quercetin as a spray reagent in inorganic thin-layer chromatography and evaluation of the chromatographed species by ring colorimetry

Summary Clean and rapid micro analytical separations of various ions in their mixed solutions have been made by the ascending TLC using quercetin (3,5,7,3,4-pentahydroxyflavone) as a spray reagent. For their evaluation, the visualized spots are scooped out with the help of Mottier gadget and transferred to the paper set on the ring oven. Separate rings were obtained for individual metal ions and the computation of their amounts is made possible by ring colorimetry, using suitable chromogenic reagents.

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Zusammenfassung Die exakte und rasche mikroanalytische Trennung verschiedener Ionen in deren Lösungsgemischen wurde durch aufsteigende Dünnschichtchromatographie unter Verwendung von Quercetin als Sprühreagens durchgeführt. Zur Auswertung wurden die sichtbar gemachten Flecken mit einem MottierGerät auf Papier übertragen und auf dem Ringofen bearbeitet. Für jedes einzelne Metall wurden verschiedene Ringe erhalten, die mit einem geeigneten Farbreagens behandelt zur kolorimetrischen Bestimmung dienten.

     

A rapid densitometric method for simultaneous quantification of gallic acid and ellagic acid in herbal raw materials using HPTLC

Gallic acid and ellagic acid are two widely occurring phenolic compounds of plant origin, to which many biological activities including anticancer and antiviral activity have been attributed. A simple HPTLC method has been developed for the simultaneous quantification of gallic acid and ellagic acid. The method was validated for precision, repeatability, and accuracy. Instrumental precision was found to be 0.083 and 0.78, and the repeatability of the method was found to be 1.07 and 1.50 (% CV) for gallic acid and ellagic acid, respectively. The accuracy of the method was checked by a recovery study conducted at two different levels and the average percentage recovery was found to be 101.02% for gallic acid and 102.42% for ellagic acid. The above method was used for the quantification of gallic acid and ellagic acid content in seeds of Abrus precatorius Linn., whole plant of Phyllanthus maderaspatensis Linn., and flowers of Nymphaea alba Linn. The proposed HPTLC method for the simultaneous quantification of gallic acid and ellagic acid was found to be simple, precise, specific, sensitive, and accurate and can be used for routine quality control of herbal raw materials and for the quantification of these compounds in plant materials.     

Monitoring solid phase synthesis reactions with electrochemical impedance spectroscopy (EIS)

This work describes the use of electrochemical impedance spectroscopy (EIS) as a means to monitor solid phase synthesis on resin beads. EIS was used to track changes during the swelling of beads in various solvents, during three typical reactions and throughout cleavage of the final product from the bead. The impedance response was investigated in a chemical reactor and was found to be faintly sensitive to the resin swelling and solvent flow. The position of the electrode within the reactor was found to be critical as polystyrene based beads float or sink dependent upon the solvent used. However, by choosing electrode position it was possible to monitor reaction progress on beads or within the bulk reactant/product mixture. Of the three typical chemical reactions studied impedance spectroscopy successfully followed two. Fitting of the impedance data to an equivalent electrical circuit provided an estimate as to the relative contribution of capacitive and resistive components to the overall response. Kinetic data from two reactions were also modelled, in both cases complex kinetics was observed, in close agreement with other studies.     

Functional group interactions of a 5-HT3R antagonist

Background  

Lerisetron, a competitive serotonin type 3 receptor (5-HT₃R) antagonist, contains five functional groups capable of interacting with amino acids in the 5-HT₃R binding site. Site directed mutagenesis studies of the 5-HT_3AR have revealed several amino acids that are thought to form part of the binding domain of this receptor. The specific functional groups on the ligand that interact with these amino acids are, however, unknown. Using synthetic analogs of lerisetron as molecular probes in combination with site directed mutagenesis, we have identified some of these interactions and have proposed a model of the lerisetron binding site.     

LC–MS Determination of Gabapentin from Human Plasma

Gabapentin is an anticonvulsant drug used for the treatment of epilepsy. It is not bound to plasma protein and is not metabolized. A high performance liquid chromatography–mass spectrometric micro method is described in this report for its determination from human plasma. Chromatography was performed on a 50 × 4.6 mm, 4 μm nitrile column and the parent ion detected in the positive ionization mode on single quadrupole analyzer (Q1MI) with atmospheric pressure ionization source. Extraction was carried out on C₁₈, 100 mg/3cc cartridge using 10 μL sample volume. The mean extraction recovery was 97% and within batch and between batch coefficients of variation were <9%. Lack of interference from endogenous substances helped in achieving a highly sensitive method without the need for monitoring fragment ions. The lowest concentration injected on column for calibration curve was 195 pg (range 0.5–64 ng). The method was applied for analysis of samples from a cross-over bio-equivalence study comparing two formulations.

     

A radioxenon detection system using PIPS and CZT

Journal of Radioanalytical and Nuclear Chemistry - This paper introduces and describes the initial characterizations of a prototype beta-gamma coincidence detection system that utilizes a PIPSBox...