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The acid-catalysed rearrangement of N-acetylhydrazobenzene was shown by thin layer chromatography to yield nine products, six of them new. In the presence of anisole the condensation products6–10 are also formed, which, just as the formation of o- and p-chloroaniline when the rearrangement is conducted in the presence of hydrochloric acid, point to the intermediate formation of phenylnitrene in the course of the benzidine rearrangement or the disproportionation. The experimental evidence of phenylnitrene in its turn supports the expandedHammick theory, on the basis of which it has been predicted.  相似文献   

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The synthesis and isolation of heptafulvene ( 1 ) and sesquifulvalene ( 2 ) is reported: Acetoxy-tropylium-fluoroborate ( 10 ) may be prepared by addition of tropone to acetyl-fluoroborate at low temperatures. The tropylium salt reacts easily with methyllithium and sodium cyclopentadienide to give the acetoxy-methyl-cycloheptatrienes 11 and the acetoxy-cyclopentadienyl-cycloheptatrienes 12 respectively. Gas-phase pyrolysis of 11 and 12 affords in remarkably good yields heptafulvene ( 1 ) and sesquifulvalene ( 2 ), which are isolated in cristalline form at low temperatures. Spectroscopic as well as chemical evidence of the title compounds is presented.  相似文献   

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Preparation, isolation, and characterization of Monoseleane and Disulphane-Diphosphonate The barium salts of monoselenane and monotellurane disulphanediphosphonate are isolated in pure state for the first time. They are characterized by analytical data and i.r. spectra.  相似文献   

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Zusammenfassung Zur Isolierung der sauren und neutralen Arzneimittel aus biologischem Material wird in den Untersuchungsgang vonStas-Otto die Dünnschicht-chromatographie zweckentsprechend eingebaut. Dieses Verfahren erlaubt die Isolierung und Erkennung der meisten praktisch in Betracht kommenden Verbindungen im Verein mit chemischen und physikalisch-chemischen Identifizierungsmethoden. Die Einfachheit der Dünnschichtchromatographie wird durch die Verwendung von nur drei Elutions- und wenigen Sprühmitteln gewahrt. Die angegebenen Rf-Werte zahlreicher Verbindungen ermöglichen dem Toxikologen eine rasche Orientierung bei der Auffindung unbekannten Substanzen.
Summary Thin layer chromatography has been appropriately incorporated into theStas Otto investigative procedure in order to isolate the acid and neutral drugs from biological material. This procedure permits the isolation and recognition of most of the compounds that come into practical consideration in connection with chemical and physico-chemical identification methods. The simplicity of thin layer chromatography is preserved by the use of only three eluants and only a few spraying agents. The stated Rf-values of numerous compounds make it possible for the toxicologists to arrive at a speedy orientation when confronted with unknown substances.


Herrn Prof. Dr.H. Lieb zu seinem 80. Geburtstag gewidmet.  相似文献   

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Isolation of antigens from foodstuffs and additivesDetection by means of immunochemical methods
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