An ESR study of some organic complexes of tetravalent vanadium

ESR results are reported for solutions and glasses containing vanadyl diethyldithiophosphate, vanadyl and vanadium diethyldithiocarbamates, and vanadium butylxanthogenate. Comparison with compounds of known structure gives the structures of these complexes.     

Comparison of fluorimetric methods of assay for 7 H-Benz(de)anthracen-7-one in airborne particulates and air pollution source effluents

Summary Various modifications of a thin-layer chromatography fluorimetric method for the determination of 7 H-benz(de)anthracen-7-one (BO) and phenalen-1-one (PO) in complex mixtures have been compared. The best modifications consisted of one-dimensional thin-layer chromatography followed by elution, evaporation, solution in trifluoroacetic acid, followed by either spectrophotofluorimetric or fluorimetric assay. In some cases a quenching agent was necessary to quench the fluorescence of the interferences. Urban atmospheres and air pollution source effluents can be analyzed by these micromethods. These methods with slight modification could be applied to the determination of the aza heterocyclic and the other ring-carbonyl compounds found in urban atmospheres and air pollution source effluents.

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Zusammenfassung Verschiedene Modifikationen einer dünnschichtchromatographischen, fluorimetrischen Methode zur Bestimmung von 7 H-Benz(de)-anthracen-7-on (BO) und Phenalen-1-on (PO) in komplexen Gemischen wurden verglichen. Am besten bewährte sich eindimensionale Dünnschichtchromatographie, nachfolgende Elution, Abdampfen, Aufnehmen in Trifluoressigsäure und schließlich Bestimmung durch Spektralfluoreszenz-oder Fluoreszenzmessung. In manchen Fällen war es nötig, die Fluoreszenz störender Substanzen mit einem geeigneten Reagens zu löschen. Stadtatmosphäre oder Quellen der Luftverunreinigung können mit diesen Mikromethoden analysiert werden. Sie eignen sich nach geringfügiger Modifikation auch zur Bestimmung von azaheterocyklischen und anderen Ring-Carbonylverbindungen in der Atmosphäre.

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Résumé On a comparé entre elles différentes modifications d'une méthode de fluorimétrie avec chromatographie en couche mince pour le dosage de la benzo-7 H anthracène-one-7 (BO) et de la phénalène-one-1 (PO) en mélanges complexes. Les modifications les meilleures ont consisté en une Chromatographie en couche mince unidimensionnelle suivie d'élution, évaporation, mise en solution dans l'acide trifluoroacétique, opérations suivies d'une recherche spectrophotofluorimétrique ou fluorimétrique. Dans certains cas, un agent d'extinction s'est montré nécessaire pour éteindre la fluorescence due aux interférences. On peut analyser par ces microméthodes les atmosphères urbaines et les écoulements sources de pollution de l'air. Ces méthodes ont pu être appliquées après légère modification au dosage des composés aza hétérocycliques et autres composés carbonyles cycliques trouvés dans les atmosphères urbaines et dans les écoulements sources de pollution de l'air.

     

5,6-Dihydro-4h-imidazole[4,5,1-i,j]quinoline derivatives

2-Alkyl(dialkyl)amino derivatives of I and their respective cyclic ammonium salts were obtained by reaction of the 2-chloro derivative of 5,6-dihydro-4H-imidazole [4,5,1-i,j ]quinoline (I) and its methiodide with amines. The eycloammonium salt was converted into 2-amino(alkylimino)-l,2-dihydro derivatives of 5. Methoxy- and methyl-substituted I readily formed 2-amino derivatives by reaction with sodium amide. Comparison of the UV spectra of the 2-amino derivative of I and its fixed tautomeric form indicates that the 2-amino derivative of I exists primarily in the amino form in dioxane and CC14.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1410–1413, October, 1970.     

Synthesis and properties of silacyclobutylsilazanes

Ammonolysis of silacyclobutanes {ie305-01} (R=Cl, CH₃) gives silacyelobutane di- and polysilazanes. Reaction of the disilazane {ie305-02} with 1-chloro-1-methyl-1-silacyelobutane at 20–80° gives a trisilyl-substituted amine {ie305-03}. Trisilyl-substituted amines with one silacyclobutyl group, are obtained by reacting silacyclobutanes {ie305-04} (R=CH₃, C₆H₅). with sodium or potassium silylamides prepared from hexamethyldisilazane. It is shown that it is possible to obtain silylamides by reacting disilazanes directly with potassium metal at 90–100°.