Darstellung und Reaktionen der 2.2.3-Trimethyl-cyclohexanon-(4)-carbonsäure

Zusammenfassung Die durch Einwirkung von konz. Schwefelsäure auf Camphandion-(2.3) in der Kälte entstehenden Substanzen werden durch Derivate charakterisiert und ihre Entstehung diskutiert.Herrn Professor Dr.Friedrich Asinger zum 60. Geburtstag gewidmet.Verstorben am 12. Dezember 1966.     

Über substituierte 1,6-Dihydro-1,3,5-triazin-2,4-diamine, 1′,5′,6′,7′-Tetrahydrospiro[cyclopentan-1,4′-cyclopentapyrimidin]-2′(3′ H)-imine und das 6-Phenyl-2,4-pyrimidindiamin

Guanidine reacts with cyclohexanone, cycloheptanone, acetone and 3-pentanone, resp., in a molar ratio 2∶1 to give the 1,3,5-triazaspiro[5.5]undeca-and [5.6]dodeca-1,3-dien-2,4-diamines3 a and3 b resp. and the 6,6-dimethylresp. diethyl-1,6-dihydro-1,3,5-triazin-2,4-diamines3 d and3 e resp. On the contrary, action of guanidine on cyclopentanone yields not3 c, but the 1′,5′,7′-tetrahydrospiro[cyclopentane-1,4′-cyclopentapyrimidine]-2′(3′H)-imines2 c, 5 c and6 c resp., which are 1∶2- and 1∶3-condensates. Phenylacetone is transformed by guanidine (1∶2) to give 6-phenyl-2,4-pyrimidindiamine (8 f). The structure of the compounds cited is proved by NMR-, IR-, and (partially) mass spectra. The different courses of the formation of3 a, b, d, e, 2 c, 5 c and6 c resp. and8 f are also discussed. The structural formulae of some additional bases, which were synthesized from guanidine and cyclopentanone, 3-pentanone and phenylacetone resp. could not be established.     

Importance of REP values when comparing the CALUX bioassay results with chemoanalyses results Example with spiked vegetable oils

Differences between chemical activated luciferase gene expression (CALUX) bioassay and chemoanalyses results are observed.This paper shows that calculations of the TEQ values using REP values instead of WHO TEF values give different results. The REP values do affect the results obtained by the CALUX technique. These differences are more marked for the dioxin like PCB compounds (CALUX TEQ values are lower than WHO TEQ values) than for the dioxin compounds (CALUX TEQ values are higher than WHO TEQ values).The CALUX results were compared with the concentrations of the congeners’ spiked into the oil.     

Beiträge zur Chemie der Enaminoketone, 2. Mitt.: Darstellung von Pyrazolo-pyridinen aus Enaminoketonen

Zusammenfassung Es wird über die Verwendung von Enaminoketonen zur Synthese von Pyrazolo[3,4-b]pyridinderivaten aus Aminopyrazolen berichtet. Mit Aminomethylencyclohexanon wird ein Pyrazolo[3,4-c]isochinolin erhalten. IR- und NMR-Spektren sowie Vergleiche mit bereits bekannten Substanzen bestätigen die Strukturen.

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The application of enaminoketones in the synthesis of pyrazolo[3,4-b]pyridine derivatives from aminopyrazoles is reported. With aminomethylenecyclohexanone a pyrazolo[3,4-c]isoquinoline is obtained. The structures are proofed by IR- and NMR-spectra and by comparison with known substances.