Mobility of trace elements in soils by thin layer chromatography - Part I

Summary Mobility of some trace elements in a soil under different conditions of leaching has been measured in terms of R_F values with the help of the thin layer method of chromatography. While the iron ions were immobile in a soil of pH 8.8, the mobility of other trace elements was also seriously affected by the presence of Na₂CO₃. Appreciable changes also occurred in the R_F values of the trace elements with the change in the nature and concentration of other leachates. Further the removal of organic matter from the soil resulted in an increase in the movement of the trace elements.

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Zusammenfassung Es wurde die Beweglichkeit von Spurenelementen in Böden gemessen und durch die R_F-Werte mit Hilfe der Dünnschichtchromatographie charakterisiert. Eisen wird bei einem pH von 8,8 unbeweglich. Auch andere Spurenelemente sind im alkalischen Bereich wenig beweglich. Die Entfernung organischer Komponenten aus dem Boden erhöht die Beweglichkeit.

     

New dioxouranium(VI) complexes with tridentate dibasic Schiff bases containing ONO donor sets

Summary Several new dioxouranium(VI) complexes with the tridentate dibasic Schiff bases derived from salicylaldehyde, 5-chloro-, 5-bromo-, 5-nitro-, 3,5-dichloro-, 4-methoxy-, 5-methoxy- and 3-ethoxysalicylaldehyde and 2-hydroxy-1-naphthaldehyde ando-aminobenzyl alcohol, have been synthesized from uranyl acetate dihydrate and the Schiff base in methanol. The complexes are of the type UO₂(AAA). MeOH (where AAAH₂ = a tridentate dibasic Schiff base). The complexes have been characterized by elemental analyses, i.r. and electronic spectra, conductance, magnetic susceptibility and molecular weight measurements. Thev (U=O) stretching frequency of the complexes occurs atca. 900 cm^–1 and the U-O distance is 1.74Å. The complexes are monomers, diamagnetic and octahedral.     

One‐pot synthesis of novel substituted pyrrolo[2,3‐d]pyrimidines using dry media

A convenient solvent‐free one‐pot synthesis of 1,3,5,7‐tetraaryl‐1,3,4,7‐tetrahydro‐2‐thio‐xopyrrolo[2,3‐d]pyrimidin‐4‐one derivatives using supported reagents under microwave irradiation is described. © 2007 Wiley Periodicals, Inc. Heteroatom Chem 18:617–621, 2007; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20355     

Synthesis and Anticancer, Antiinflammatory,and Analgesic Activity Evaluation of Some Sulfa Drug and Acridine Derivatives

 Various sulfa drugs were condensed with 4-isothiocyanato-4-methyl-2-pentanone at pH∼3–5 by refluxing in methanol to give various substituted mercaptopyrimidines. On condensation with 9-chloro-2-substituted or -unsubstituted acridines, sulfathiazole gave the corresponding condensed products. N-Ethylaminoadenosine reacted with 9-chloroacridine to the coupled product. Condensation of sulfathiazole with 9-isothiocyanato-2,4-substituted or -unsubstituted acridines afforded the corresponding condensed compounds. The structures of all synthesized compounds were confirmed by spectroscopic methods. Anticancer, antiinflammatory, and analgesic activities of all compounds were investigated.     

UPLC‐MS/MS assay for the simultaneous quantification of carvedilol and its active metabolite 4′‐hydroxyphenyl carvedilol in human plasma to support a bioequivalence study in healthy volunteers

An ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS) method has been developed for the simultaneous determination of carvedilol and its pharmacologically active metabolite 4′‐hydroxyphenyl carvedilol in human plasma using their deuterated internal standards (IS). Samples were prepared by solid‐phase extraction using 100 μL human plasma. Chromatographic separation of analytes was achieved on UPLC C18 (50 × 2.1 mm, 1.7 µm) column using acetonitrile‐4.0 mm ammonium formate, pH 3.0 adjusted with 0.1% formic acid (78:22, v/v) as the mobile phase. The multiple reaction monitoring transitions for both the analytes and IS were monitored in the positive electrospray ionization mode. The method was validated over a concentration range of 0.05–50 ng/mL for carvedilol and 0.01‐10 ng/mL for 4′‐hydroxyphenyl carvedilol. Intra‐ and inter‐batch precision (% CV) and accuracy for the analytes varied from 0.74 to 3.88 and 96.4 to 103.3% respectively. Matrix effect was assessed by post‐column analyte infusion and by calculation of precision values (coefficient of variation) in the measurement of the slope of calibration curves from eight plasma batches. The assay recovery was within 94–99% for both the analytes and IS. The method was successfully applied to support a bioequivalence study of 12.5 mg carvedilol tablets in 34 healthy subjects. Copyright © 2013 John Wiley & Sons, Ltd.     

Synthesis and properties of 3,4-dioxythiophene and 1,4-dialkoxybenzene based copolymers via direct C?H arylation: Dopant-free hole transport material for perovskite solar cells

Direct C H arylation coupling reaction has gained significant importance in synthesis of conjugated polymers for organic electronic applications. We report here a facile and straightforward method called “direct C H arylation” reaction to synthesize conjugated 3,4-dioxythiophene and 1,4-dialkoxybenzene based copolymers as hole transport material (HTM) for perovskite solar cells. Two electron-rich conjugated polymers P1-2 were synthesized, in which 1,4-dibromo-2,5-bis(dodecyloxy)benzene and 3,4-dialkoxy-thiophene units were used for polymerization. The resulting polymers were characterized and exhibited high solubility in organic solvents. Electrochemical and optical characterizations were carried out by cyclic voltammetry and UV–Vis–NIR absorption spectroscopy and found that these polymers show higher-lying HOMO energy levels with wide band gap. Density functional theory calculation was performed on these polymers ( P1-2 ) and correlated with our experimental results. Finally, perovskite solar cells were fabricated by solution-processable deposition of P1-2 as dopant-free HTM with device geometry ITO/SnO₂/Perovskite/HTM( P1 / P2 )/Ag and achieved a maximum power conversion efficiency of 5.28%. This study provides information on designing and simple preparation by direct C H arylation reaction of higher-lying HOMO energy level polymer as HTM for perovskite solar cells.     

Synthesis for Pyridopyrimidinones

An improved clean methodology has been developed for the synthesis of pyrido[2,3‐d]pyrimidin‐4‐ones through a simple one‐pot reaction of chalcones, ketones, and ammonium acetates via a [3+2+1] ring annulation. This dry media methodology, where the three components absorbed over solid inorganic support under microwave irradiation, afforded the desired product in a short reaction time.