An efficient one-pot three-component synthesis and antimicrobial evaluation of tetra substituted thiophene derivatives

A convenient one-pot three-component method for the preparation of tetra-substituted thiophene derivatives has been developed. Reaction of acetyl acetone 1, phenyl isothiocynate 2 and 2-chloromethyl derivatives 3a–3c in the presence of potassium carbonate afforded the target compounds, namely ethyl2-(4-acetyl-3-methyl-5-(phenylamino)thiophen-2-yl)-2-oxoacetate derivatives 4a–4e, ethyl 3-(4-acetyl-3-methyl-5-(phenylamino)thiophen-2-yl)-3-oxopropanoate derivatives 4f–4i, di((4-acetyl-3-methyl-5-phenylamino)thiophen-2-yl)ketone derivatives 4j–4n in reasonable overall yields. The synthesized compounds were screened for antimicrobial activity. The detailed synthesis, spectroscopic data and antimicrobial activities of synthesized compounds were reported.     

Single molecule conformational analysis of the biologically relevant DNA G-quadruplex in the promoter of the proto-oncogene c-MYC

Single molecule fluorescence spectroscopy has been employed to resolve the conformational heterogeneity, hybridization kinetics and study mutational effects on the c-MYC promoter G-quadruplex.     

Experimental investigation and simulation of hollow fiber membrane process for SF6 recovery from GIS

In this present study, polyethersulfone hollow fiber membrane was used to recover sulfur hexafluoride (SF₆) from gas‐insulated switchgear (GIS). SF₆, N₂ pure gas and mixed gas (12.5 vol.% of SF₆) experiment was initiated to observe permeation behavior according to temperature and pressure difference and retentate flow rate. Scanning electron microscopy was used to investigate the morphological characteristics and the structure of asymmetric hollow fibers. The permeation rates of SF₆ and N₂ were measured by the variable pressure method. As a result, permeance of N₂ was 9.5–16.3 GPU, and selectivity of N₂/SF₆ was 10.5–13.3. Moreover, the concentration of SF₆ in the retentate stream reached to 99.2% by the control of the operating condition. Based on the experimental results, tree‐stage membrane process was designed using simulation program. As a result, demanded membrane area reduced about 74% according to operating condition difference. Copyright © 2013 John Wiley & Sons, Ltd.     

Asymmetric Synthesis of (R)-Fluoxetine: A Practical Approach Using Recyclable and in-situ Generated Oxazaborolidine Catalyst

A practical route for the synthesis of (R)-fluoxetine•HCl (ee＝96%) in 56% overall yield was described. The key intermediate (R)-3-chloro-1-phenyl-1-propanol was obtained by the asymmetric reduction of prochiral 3-chloropropiophenone using in-situ generated oxazaborolidine catalyst derived from (S)-α,α-diphenylprolinol. The chiral procatalyst (S)-α,α-diphenylprolinol was recovered quantitatively and recycled. An improved practical synthesis of (S)-α,α-diphenylprolinol was also discussed.     

A facile and rapid access towards the synthesis of 2,3-dihydroquinazolin-4(1H)-ones

An efficient synthetic route for 2,3-dihydroquinazolin-4(1H)-ones using 2-morpholinoethanesulfonic acid as a potential and new organocatalyst is described. The developed synthetic protocol represents a novel and very simple route for the preparation of 2,3-dihydroquinazolin-4(1H)-one derivatives. In addition, microwave irradiation technique is successfully implemented for carrying out the reactions in shorter reaction times.     

Green multicomponent reaction for synthesis of trisubstituted pyrroles in ionic liquid [bmim]BF<Subscript>4</Subscript>

2,4,5-Trisubstituted pyrrole derivatives were efficiently synthesized by one-pot condensation of 1,3-diones, α-bromoacetophenones, and ammonium acetate in ionic liquid [bmim]BF₄. The new synthetic method offers multisubstituted pyrroles with the advantages of mild reaction conditions, operational simplicity, higher yield, and environmental friendliness.     

Hydrothermal Assisted Synthesis of Micro-Bricks Shaped WO3 for Electrochemical Oxidation of Paracetamol: A Microstructured Paracetamol Sensor

Russian Journal of Electrochemistry - A micro-bricks shaped tungsten oxide (WO3) was prepared by hydrothermal method. The prepared material was characterized by field emission scanning electron...     

2-Nitrobenzaldehyde Thiocarbohydrazone Assisted Precise Extraction Spectrophotometric Method for the Determination of Ruthenium(III) in Alloy and Catalysts

A simple, rapid, selective, sensitive and reliable extractive spectrophotometric method was developed for the determination of ruthenium(III) using 2-nitrobenzaldehyde thiocarbohydrazone (2-NBATCH) as a chromogenic chelating ligand. The ruthenium(III)?2-NBATCH complex is formed in aqueous acetic acid media (0.7 M) containing an organic solvent after 5 min heating on a water bath. The red colored complex is extracted into 1,2-dichloroethane and absorbance is measured at 445 nm against reagent blank. The Beer’s law is obeyed within 1?6 g/mL of ruthenium(III), the optimum concentration range was 2?5 g/mL of ruthenium(III) evaluated by Ringbom’s plot. Molar absorptivity and Sandell’s sensitivity of complex were 1.41 × 10⁴ L/mol/cm and 0.0075 μg/cm², respectively. The stoichiometry of complex was 1: 3 established from Job’s method of continuous variation, molar ratio method and logarithmic slope method. The proposed method was applied for determination of ruthenium(III) in binary and ternary, synthetic mixtures corresponding to fission product elements alloy and ruthenium(III) catalysts.     

Chromatographic determination of itopride hydrochloride in the presence of its degradation products

Two sensitive and reproducible methods are described for the quantitative determination of itopride hydrochloride (IH) in the presence of its degradation products. The first method is based on HPLC separation on a reversed phase Kromasil column [C18 (5-microm, 25 cm x 4.6 mm, ID)] at ambient temperature using a mobile phase consisting of methanol and water (70:30, v/v) adjusted to pH 4.0 with orthophosphoric acid with UV detection at 258 nm. The flow rate was 1.0 mL per min with an average operating pressure of 180 kg/cm2. The second method is based on HPTLC separation on silica gel 60 F254 using toluene:methanol:chloroform:10% ammonia (5.0:3.0:6.0:0.1, v/v/v/v) as mobile phase at 270 nm. The analysis of variance (ANOVA) and Student's t-test were applied to correlate the results of IH determination in dosage form by means of HPLC and HPTLC methods. The drug was subjected to acid and alkali hydrolysis, oxidation, dry heat, wet heat treatment, UV, and photodegradation. The proposed HPLC method was utilized to investigate the kinetics of the acidic, alkaline, and oxidative degradation processes at different temperatures and the apparent pseudo-first-order rate constant, half-life, and activation energy were calculated. In addition the pH-rate profile of degradation of IH in constant ionic strength buffer solutions in the pH range 2-11 was studied.