Electrochemical Evaluation of Diketopyrrolopyrrole Derivatives for Nonaqueous Redox Flow Batteries

Redox flow batteries (RFBs) employing nonaqueous electrolytes could potentially operate at much higher cell voltages, and therefore afford higher energy and power densities, than RFBs employing aqueous electrolytes. The development of such high-voltage nonaqueous RFBs requires anolytes that are electrochemically stable, especially in the presence of traces of oxygen and/or moisture. The inherent atmospheric reactivity of anolytes mandates judicious molecular design with high electron affinity and electrochemical stability. In this study, diketopyrrolopyrrole (DPP)-based TDPP-Hex-CN₄ is proposed as a stable redox-active molecule for anolytes in nonaqueous organic RFBs. We demonstrate organic RFBs using TDPP-Hex-CN₄ as anolyte with unisol blue (UB) 1,4-bis(isopropylamino)anthraquinone and 1,4-di-tert-butyl-2,5-bis(2-methoxyethoxy)benzene (DBBB) as catholytes. Cyclic voltammetry measurements with scans repeated over 200 cycles were performed to establish the electrochemical stability of the redox pairs. Symmetric flow-cell studies show that TDPP-Hex-CN₄ exhibits stable capacity up to 700 cycles. Redox flow cells employing TDPP-Hex-CN₄ /UB and TDPP-Hex-CN₄/DBBB as redox pairs demonstrate that DPP derivatives are propitious materials for anolytes in all organic nonaqueous RFBs.     

Green Approach to the Synthesis of New Indole and Benzimidazole Analogs and Their Biological Evaluation

Russian Journal of Organic Chemistry - To obtain new lead compounds with potent antimicrobial and antioxidant activities, new indole analogs containing various heterocyclic moieties were...     

Microwave-Assisted Synthesis of Some Indole and Isoniazid Derivatives as Antitubercular Agents and Molecular Docking Study

Russian Journal of Organic Chemistry - An efficient and expeditious microwave-assisted synthesis of isoniazid derivatives from various indole-3-carbaldehydes, phenols, and isoniazid via...     

Review of the synthesis,characterization, and properties of LaAlO3 phosphors

In this review different methods of preparing lanthanum aluminate (LaAlO₃) phosphors are discussed. The molten salt method, the combustion method, the sucrose method, and the coprecipitation technique are the best methods for preparing LaAlO₃ phosphors with small particle size and high surface area by low-temperature synthesis. LaAlO₃ usually has a rhombohedral structure. It has good dielectric properties and, hence, is regarded as an attractive alternative to SiO₂ in microelectronic devices. LaAlO₃ phosphors have excellent chemical and thermal stability, mechanical durability, and exploitable optical and electronic properties, leading to a wide range of potential applications. LaAlO₃ phosphors doped with rare-earth ions have luminescence properties and can, hence, be used in optical display systems.     

Semi-synthesis of a novel hybrid isoxazolidino withaferin via chemoselective and diastereoselective 1,3-dipolar nitrone cycloaddition reaction

Abstract

A facile, atom-economic synthesis of isoxazilidino withaferin, a novel hybrid of withaferin A, has been accomplished via two-step reaction of nitrone synthesis followed by nitrone 1,3-dipolar cycloaddition. The reaction is highly chemoselective (preferential reaction only on one of the two double bonds present on withaferin A) and diastereoselective affording exclusively the cis-fused products. The structure was determined by detailed analysis of 1D, 2D NMR and mass spectral data.     

Simultaneous Estimation of Atorvastatin Calcium, Ramipril and Aspirin in Capsule Dosage Form by RP-LC

A simple, sensitive, precise and accurate reversed phase liquid chromatographic method has been developed for the simultaneous estimation of atorvastatin (AT) calcium, ramipril (RA) and aspirin (AS) from capsule dosage form. The method was developed using a Phenomenex Luna C₁₈ (250 mm, 4.6 mm i.d., 5 µm) column with a mobile phase consisting of 0.1%, orthophosphoric acid buffer:acetonitrile:methanol (45:50:5 v/v/v), pH 3.3, at a flow rate of 1 mL min^?1. Detection was carried out with ultra-violet detection at 210 nm. The retention times were about 12.19, 2.35, and 3.95 min for AT calcium, RA and AS, respectively. The developed method was validated for linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. The linearity ranges were 1–6 µg mL^?1 for AT calcium, 0.5–3 µg mL^?1 for RA and 7.5–45 µg mL^?1 for AS with mean recoveries of 100.59 ± 0.68, 100.62 ± 0.83 and 100.49 ± 0.73% for AT calcium, RA and AS, respectively. Limit of detection obtained were 29.85 ng mL^?1 for AT calcium, 4.71 ng mL^?1 for RA and 85.13 ng mL^?1 for AS. Impurity of salicylic acid was found in capsule dosage form at the retention time of about 4.84 min. The proposed method can be used for the estimation of these drugs in combined dosage forms.     

Optimization of biodiesel production in a hydrodynamic cavitation reactor using used frying oil

The present work demonstrates the application of a hydrodynamic cavitation reactor for the synthesis of biodiesel with used frying oil as a feedstock. The synthesis involved the transesterification of used frying oil (UFO) with methanol in the presence of potassium hydroxide as a catalyst. The effect of geometry and upstream pressure of a cavitating orifice plate on the rate of transesterification reaction has been studied. It is observed that the micro level turbulence created by hydrodynamic cavitation somewhat overcomes the mass transfer limitations for triphasic transesterification reaction. The significant effects of upstream pressure on the rate of formation of methyl esters have been seen. It has been observed that flow geometry of orifice plate plays a crucial role in process intensification. With an optimized plate geometry of 2 mm hole diameter and 25 holes, more than 95% of triglycerides have been converted to methyl esters in 10 min of reaction time with cavitational yield of 1.28 × 10^?3 (Grams of methyl esters produced per Joule of energy supplied). The potential of UFO to produce good quality methyl esters has been demonstrated.     

MSn,LC‐MS‐TOF and LC‐PDA studies for identification of new degradation impurities of bupropion

Three new degradation impurities of bupropion were characterized through high performance liquid chromatography coupled to photodiode array detection and to time‐of‐flight mass spectrometry. Bupropion was subjected to the ICH prescribed stress conditions. It degraded to seven impurities (I–VII) in alkaline hydrolytic conditions which were optimally resolved on an XTerra C₁₈ column (250 × 4.6 mm, 5 µm) with a ternary mobile phase comprising ammonium formate (20 mm , pH 4.0), methanol and acetonitrile (75:10:15, v/v). The degradation impurities (III–V and VII) were characterized on the basis of mass fragmentation pattern of drug, accurate mass spectral and photodiode array data of the drug and degradation impurities. Compound V was found to be a known degradation impurity [1‐hydroxy‐1‐(3‐chlorophenyl)propan‐2‐one], whereas III, IV and VII were characterized as 2‐hydroxy‐2‐(3′‐chlorophenyl)‐3,5,5‐trimethylmorpholine, (2,4,4‐trimethyl‐1,3‐oxazolidin‐2‐yl)(3‐chlorophenyl)‐methanone and 2‐(3′‐chlorophenyl)‐3,5,5‐trimethylmorphol‐2‐ene, respectively. Compound III was a known metabolite of the drug. This additional information on the degradation impurities can help in the development of a new stability‐indicating assay method to monitor the stability of the drug product during its shelf‐life as well as in development of a drug product with increased shelf‐life. Copyright © 2013 John Wiley & Sons, Ltd.     

The First Stereoselective Total Synthesis of a Naturally Occurring Bioactive Diarylheptanoid, (3R,6E)‐1,7‐Bis(4‐hydroxyphenyl)hept‐6‐en‐3‐ol,through Two Different Approaches

The stereoselective total synthesis of a naturally occurring bioactive diarylheptanoid, (3R,6E)‐1,7‐bis(4‐hydroxyphenyl)hept‐6‐en‐3‐ol, has been accomplished starting from 4‐hydroxybenzaldehyde through two different approaches involving Wittig olefination, hydrolytic kinetic resolution of a racemic epoxide, and olefin cross‐metathesis reaction as the key steps.     

Multiporphyrin arrays on cyclophosphazene scaffolds: synthesis and studies

The stable and robust cyclotriphosphazene and cyclotetraphosphazene rings were used as scaffolds to prepare hexa- and octaporphyrin arrays by treating N(3)P(3)Cl(6) and N(4)P(4)Cl(8), respectively, with 5-(4-hydroxyphenyl)-10,15,20-tri(p-tolyl)porphyrin (N(4) core) or with its thiaporphyrin analogues (N(3)S and N(2)S(2) cores) in THF in the presence of Cs(2)CO(3) under simple reaction conditions. Thiaporphyrins were examined in addition to the normal porphyrin to tune the electronic properties of the resultant arrays. Observation of the molecular ion peaks in the mass spectra confirmed the molecular structures of the arrays. 1D and 2D NMR techniques were employed to characterize the multiporphyrin arrays in detail. The (1)H NMR spectra of the multiporphyrin arrays each show a systematic set of signals, indicating that the porphyrin units are arranged in a symmetrical fashion around the cyclophosphazene rings. All signals in the (1)H NMR spectra were assigned with the aid of COSY and NOESY experiments. The protons of each porphyrin unit are subject to upfield and downfield shifts because of the ring-current effects of neighboring porphyrin units. Optical, electrochemical, and fluorescence studies of the arrays indicated that the porphyrin units retain their independent ground- and excited-state characteristics. Cu(II) and Ni(II) derivatives of hexaporphyrin and octaporphyrin arrays containing N(4) porphyrin units and N(3)S porphyrin units were synthesized, and complete metalation of the arrays was confirmed by their mass spectra and by detailed NMR characterization of the Ni(II) derivatives of hexa- and octaporphyrin arrays containing N(4) porphyrin units. Electrochemical studies indicated that Cu(II) and Ni(II) ions present in the thiaporphyrin units of the arrays can be stabilized in the +1 oxidation state, which is not possible with arrays containing normal porphyrin units.