The chelation of poly(0-isophthaloylisophthalamide oxime) (1) with copper(I1) ions was carried out under various conditions and with different copper(I1) compounds. The effect of the chelation conditions on the metal content of the chelated polymer was studied. All polymers were characterized by IR spectra, solubilities, thermal analysis, and X-ray diffraction. It was found that the copper(l1) chelates of 1 are thermally less stable than the cyclized prepolymer. A soluble chelate polymer was obtained by the reaction of the polymeric ligand with the o-phenylenediamine-copper(1I) complex.
ZUSAMMENFASSUNG:Die Chelatbildung von Poly(0-isophthaloylisophthalamidoxim) ( I ) mit Kupfer(l1)-Ionen wurde unter verschiedenen Bedingungen und mit verschiedenen Kupfer(I1)-Verbindungen untersucht. Der EinfluB der Chelatisierungsbedingungen auf die Metallkonzentration der Chelat-Polymeren wurde gepriift. Alle Polymere wurden durch IR Spektrum, Loslichkeit, Thermoanalyse und Rontgen-Diffraktion charakterisiert. Es wurde gefunden, daB die Kupfer(I1)-Chelate von I thermisch weniger stabil sind als das cyclisierte Prepolymer. Ein losliches Chelat-Polymer wurde durch Reaktion des polymeren Liganden mit dem o-Phenylendiamin-Kupfer(I1)-Komplex hergestellt.
The chromatographical characteristics of 1,5-anhydroglucitol in thin-layer chromatograms can be studied using the customary carbohydrate solvents. Both hydrogen peroxide and sodium metaperiodate oxidation reactions were tested in order to find a specific colour reaction for the detection of the compound. 1,5-anhydroglucitol was readily converted by periodate into an intermediate product which produced an intense orange-red colour with diphenylamine aniline reagent. According to data obtained from periodate oxidation, IR spectroscopy and mass fragmentography, the intermediate product was a dialdehyde compound with a C6 structure, possibly formed through cleavage at C2-C3. The formation of a compound of this kind without chain cleavage in the periodate oxidation of C6 carbohydrates is uncommon. Periodate oxidation followed by diphenylamine-aniline reaction affords a sensitive and specific method for the detection of 1,5-anhydroglucitol.
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