Synthesis, characterization, biocide and toxicological activities of di-n-butyl- and diphenyl-tin(IV)-salicyliden-beta-amino alcohol derivatives

The one pot reaction of salicylaldehyde 1, beta-amino alcohols 2a-2c, and di-n-butyltin(IV) oxide 3a or diphenyltin(IV) oxide 3b produced five diorganotin(IV) compounds, 4a-4c, 5a, and 5c, in good yields. All compounds were characterized by IR, (1)H, (13)C, and (119)Sn NMR spectroscopy, and elemental analysis; furthermore, compounds 4b, 4c, 5a, and 5c were characterized by X-ray diffraction analysis. After the structural characterization, all of the compounds were tested in vitro against Bacillus subtilis (Gram-positive, strain ATCC 6633), Escherichia coli (Gram-negative, strain DH5alpha), Pseudomonas aeruginosa (Gram-negative, strain BH3), Desulfovibrio longus (strain DSM 6739), and Desulfomicrobium aspheronum (strain DSM 5918) to assess their antimicrobial activity. Compounds 4 and 5 demonstrated a wide range of bactericidal activities against the tested aerobic (one Gram-positive and two Gram-negative subtypes) and anaerobic bacteria (two sulfate-reducing bacteria, SRB). Compound 5 had better bactericidal performances than compound 4. For all of the compounds, the acute toxicity was measured using luminescent bacteria toxicity (LBT-Microtox) tests to track their further environmental impact. According to these results and in order to fulfill environmental regulations, the toxicity of the compounds studied herein can be modulated through the proper selection of the disubstituted tin(IV) moiety.     

Elemental speciation by chromatographic separation with inductively coupled plasma mass spectrometry detection

Separation techniques coupled to inductively coupled plasma mass spectrometry (ICP-MS) is reviewed. ICP-MS technique is described briefly. Coupling of the different separation techniques are described, together with the most common applications used for each technique that has been described in the literature. An overview for the future of separation techniques coupled to ICP-MS with regard to elemental speciation is discussed.     

Evaluation of Ptitsyn-Eizner λ parameter in dilute solutions of poly(N-vinylcarbazole) and its variation in conformational transitions of poly(methyl methacrylate)

The Ptitsyn-Eizner λ flexibility parameter for poly(N-vinylcarbozole) solutions under theta conditions has been found to be 6.31, demonstrating the rigidity imparted to the polymer chain by the carbazole group. A study has been made of the variation of this parameter with solvent and temperature. A study has been made of the variation of λ in a conformational transition of poly(methyl methacrylate).     

Synthesis of 4-thia analogues of isoquinoline alkaloids

Summary (±)-4-Thiacarnegin (3) was synthesized by reaction of 6,7-dimethoxy-3-methyl-2H-1,3-benzothiazinium iodide (2) with methyl magnesium iodide, thereby opening a new synthetic route to 4-substituted dihydro-2H-1,3-benzothiazines. Compound3 was also obtained by reduction of 6,7-dimethoxy-3,4-dimethyl-2H-1,3-benzothiazinium iodide (5). In a similar way, reduction of the quaternary salts9 a–c afforded the (±)-4-thia analogues of cryptostilin-I, -II and -III (10 a–c). The isomers of the former compounds (12 a–c) were also synthesized by reduction of the 4H-1,3-benzothiazinium salts11 a–c.

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Synthese von 4-Thiaanalogen von Alkaloiden mit Isochinolingerüst

Zusammenfassung Aus 6,7-Dimethoxy-3-methyl-2H-1,3-benzothiaziniumjodid (2) wurde mit Methylmagnesiumjodid (±)-Thiacarnegin (3) dargestellt. Diese Reaktion bietet ein neues Verfahren für die Synthese von 4-substituierten Dihydro-2H-1,3-benzothiazinen.3 wurde auch durch Reduktion von 6,7-Dimethoxy-3,4-dimethyl-2H-1,3-benzothiaziniumjodid (5) erhalten. Die Reduktion der quartären Ammoniumsalze9 a–c ergab ebenfalls die Cryptostillin I-, II-, III-(±)-4-thiaanalogen Verbindungen (10 a–c). Reduktion der 4H-1,3-Benzothiazinium-Salze11 a–c lieferte die entsprechenden Isomeren12 a–c der obengenannten Verbindungen.

     

Continuous determination of carbon dioxide evolved during thermal decomposition reactions

A simple device suitable for continuous monitoring of carbon dioxide evolved during thermal decomposition reactions is described. Carbon dioxide is transported by a carrier gas through the device connected to thermoanalytical equipment and absorbed by soda lime reagent. The reaction heat released is linearly proportional to the amount of carbon dioxide absorbed.     

New glycidyl ester compounds containing a preformed imide ring—I

The synthesis of the new esterglycidyl compounds produced by condensation of bis-carboxyimides with a large excess of epichlorohydrin were reported. To define the optimal conditions of condensation the process with monofunctional compounds were studied at first. For all synthesis, yield and epoxide and chlorine contents were found. The structure of glycidyl esters was determined by elementary analysis, IR and ¹H and ¹³C NMR spectra. The physical properties were also defined.     

Rapid spectrophotometric determination of chlorate with dimedone bisthiosemicarbazone monohydrochloride

Summary Dimedone bisthiosemicarbazone monohydrochloride has been examined to evaluate its usefulness as a reagent for rapid and sensitive Spectrophotometric determination of chlorate (0.5–5.0 ppm) by oxidation of the reagent in 70% perchloric acid medium and measurement of the yellow product. The molar absorptivity at 417 nm is 1.86×10⁴ l·mole^–1·cm^–1. The relative standard deviation is 1.6% for 2.5 ppm of chlorate.

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Spektropbotometrische Bestimmung von Chlorat mit Dimedonbisthiosemicarbazon-monocblorhydrat (I)

Zusammenfassung Die Verwendbarkeit von I als Reagens für die rasche und empfindliche spektrophotometrische Bestimmung von 0,5–5,0 ppm Chlorat durch Oxydation von I in 70%iger Perchlorsäure und Messung des gelben Reaktionsproduktes wurde untersucht. Die molare Absorptivität bei 417 nm beträgt 1,86×10⁴ l·mol^–1·cm^–1. Die relative Standardabweichung beträgt 1,6% für 2,5 ppm Chlorat.

     

Cycloaddition chemistry of 2-vinyl-substituted indoles and related heteroaromatic systems

[reaction: see text] The intramolecular Diels-Alder cycloaddition reaction (IMDAF) of several N-phenylsulfonylindolyl-substituted furanyl carbamates containing a tethered pi-bond on the indole ring were examined as an approach to the iboga alkaloid catharanthine. Only in the case where the tethered pi-bond contained two carbomethoxy groups did the [4 + 2]-cycloaddition occur. Push-pull dipoles generated from the Rh(II)-catalyzed reaction of diazo imides, on the other hand, undergo successful intramolecular 1,3-dipolar cycloaddition across both alkenyl and heteroaromatic pi-bonds to provide novel pentacyclic compounds in good yield and in a stereocontrolled fashion. The facility of the cycloaddition was found to be critically dependent on conformational factors in the transition state. Ligand substitution in the rhodium(II) catalyst markedly altered the product ratio between [3 + 2]-cycloaddition and intramolecular C-H insertion. The variation in reactivity reflects the difference in electrophilicity between the various rhodium carbenoid intermediates. Intramolecular C-H insertion is enhanced with the more electrophilic carbene generated using Rh(II) perfluorobutyrate.     

Liquid-vapor interface of square-well fluids of variable interaction range

Properties of the liquid-vapor interface of square-well fluids with ranges of interaction lambda=1.5, 2.0, and 3.0 are obtained by Monte Carlo simulations and from square-gradient theories that combine the Carnahan-Starling equation of state for hard spheres with the second and third virial coefficients. The predicted surface tensions show good agreement with the simulation results for lambda=2 and for lambda=3 in a temperature range reasonably close to the critical point, 0.8相似文献   

Spectrofluorimetric determination of moxifloxacin in tablets, human urine and serum

A spectrofluorimetric method to determine the antibiotic moxifloxacin is proposed and was applied to pharmaceuticals, human urine and serum. The fluorimetric method allows the determination of 30-300 ng mL-1 moxifloxacin in aqueous solution containing phosphoric acid-phosphate buffer (pH 8.3) with lambda exc = 287 nm and lambda em = 465 nm. Detection and quantification limits were 10 and 30 ng mL-1, respectively, with a relative standard deviation (n = 10) of 2%. This method was applied to the determination of moxifloxacin in three Spanish commercial pharmaceutical formulations. Another variant of the method in micellar medium allows the direct measurement of moxifloxacin in human serum and urine by standard additions. The enhanced fluorescence of moxifloxacin in 8 mM sodium dodecyl sulfate (SDS) solution at pH 4.0 (acetic acid-acetate buffer) for lambda exc = 294 nm and lambda em = 503 nm shows the same linear range as the aqueous method with a 25% lower slope (with detection and quantification limits of 15 and 60 ng mL-1, respectively, and a relative standard deviation of 1.3%), but permits the background fluorescence for urine and serum blanks to be minimized. Hence, sufficient sensitivity is reached to determine therapeutic concentrations of the drug in urine (average recovery 102 +/- 2%) and serum (average recovery 105 +/- 2%) samples.