Alizarin-s,a reagent for thorium. a gravimetric,colorimetric, and spectrophotometric study

The claim of Beck in the use of alizarin-S for separating cerite earths from thorium could not be substantiated. Detailed conditions for estimating from 0.0095 to 6.3 mg of thorium dioxide in 50 ml of solution by the method of Rao and Murthy are described. The absorption characteristics of alizarin-S and its-thorium complex have been studied in their dependance on pH. The thorium complex has been shown by adopting different optical methods to correspond to Th-Al-S (a stoichiometric ratio of 1:1) which is also confirmed from gravimetric analyses. The dissociation coefficient of the complex at pH 2.7 has been computed to be less than 1.10^-8.     

Peroxide chemistry of triaryl-substituted imidazoles. Fenflumizole, a non-steroidal, anti-inflammatory agent.

Fenflumizole, [2-(2,4-difluorophenyl)4,5-bis(4-methoxyphenyl)imidazole] is a nonsteroidal, anti-inflammatory analgesic. It reacts quantitatively with 1O2 forming 2-(2,4-difluorophenyl)-4-hydroperoxy-4,5-bis(4-methoxyphenyl)imidazole in a reversible reaction. In ethanol solution at ambient temperatures, the peroxide regenerates parent fenflumizole and 1O2 together with minor quantities of other products. The structures of those products point to the intermediacy of a 1,3-endoperoxide and a dioxetane. These observations may be relevant to the biological activity of fenflumizole.     

Polyimidines,a new class of polymers. II. Polyhexamethylenetetraphenyldithiopyromellitimidine

Polyimidines have been shown to be soluble, thermally stable polymers. In searching for an alternate synthetic method the thio analog of this system has been discovered. The brightly colored (red-orange) perthio derivatives of 3,3-diphenylphthalide and 3,3,5,5-tetraphenyipyromellitide were synthesized from their oxo analogs with P₂S₅. The model compound thioimidines were synthesized by reacting 3,3-diphenyldithiophthalide with aniline and with 1,6-hexane diamine and by reacting 3,3,5,5-tetraphenyltetrathiopyromellitide with aniline and n-hexylamine. The polymerization of tetraphenyltetrathiopyromellitide occurred readily with 1,6-hexanediamine in boiling carbon tetrachloride with complete cyclization. This reaction gave an 80% yield with inherent viscosities up to 0.89 and molecular weights up to approximately 11,000. Thermogravimetric analysis showed a 2% weight loss at 200°C and 10% weight loss at 300°C with rapid decomposition above 300°C. Although the polythioimidine was less thermally stable than its oxo analog, it was much more soluble in common solvents (aromatic and chlorinated aliphatic hydrocarbons) and more readily synthesized in higher yield.     

Oxidative coupling in 4a,9-diaza-1,2,4a,9a-tetrahydrofluorene derivatives. 2. Synthesis of methylenequinoneimines

The oxidative coupling of 4a,9-diaza-1,2,4a,9a-tetrahydro-9H-fluorene derivatives with methylene-active compounds in the presence of MnO₂ leads to substituted (at the methylene group) 6-methylene-4a,9-diaza-1,2,4a,9a-tetrahydro-6H-fluorene derivatives. The corresponding 2,2-disubstituted 5-dicyanomethylene-3,5-dihydrobenzimidozoles were obtained in the reaction of 2,2-disubstituted benzimidazolines with malonitrile in the presence of MnO₂.See [1] for Communication 1.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 779–785, June, 1990.     

Microbial products. II. Granaticinic acid,a new antibiotic from a thermophilic streptomycete

Streptomyces sp. XT-11989 produces a mixture of two antibiotics with litmus-like indicator properties. One of them was shown to be identical with granaticin, the other was identified as [1S,3S,4S,7R,9R,10S,13R]-4,7,9,10-tetrahydro-5,12-dioxo-4, 6,10,11,13-pentahydroxy-1,9-dimethyl-(1H,3H)-7,10-ethanonaphtho[2,3-c: 6,7-c]dipyran-3-acetic acid and termed granaticinic acid. Microbial production and nuclear magnetic resonance data of these antibiotics are discussed and the antibacterial properties of the antibiotics are compared.

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Mikrobielle produkte. II. Granaticinsäure, ein neues Antibiotikum von einem thermophilen Streptomyceten

Zusammenfassung Der Streptomycetenstamm XT-11989 produziert eine Mischung von zwei Antibiotika mit Lakmus-ähnlichen Indikatoreigenschaften. Eines dieser Antibiotika erwies sich als Granaticin, das andere wurde als [1S,3S,4S,7R,9R,10S,13R]-4,7,9,10-tetrahydro-5,12-dioxo-4,6,10,11,13-pentahydroxy-1,9-dimethyl-(1H,3H)-7,10-ethanonaphto[2,3-c: 6,7-c]dipyran-3-essigsäure identifiziert und Granaticinsäure benannt. Mikrobiologische Produktion und Kernresonanzdaten dieser antibiotika werden besprochen und ihre antibakteriellen Eigenschaften verglichen.

     

Spirophosphoranes a liaison P-OH. Synthese,tautomerie

Spirophosphoranes with a P-OH bond have been prepared as free acid (compound 5c), triethylammonium salts (compounds 2c–6c), or adducts $\text{1}\text{1}$ with DMF (compounds 5c and 6c). The ionic feature of triethylammonium salts of compounds 1c–6c, shows that these Spirophosphoranes are relatively strong Brønsted's acids. Tautomeric equilibrium phosphoric ester—phosphorane with a P-OH bond [Scheme 9), shown in many cases, has been studied by means of ³¹PN, MRspectroscopy. Influence of factors ruling this equilibrium is analysed. Some elements of dynamic stereochemistry are examined.     

Heteroaromatic alkaloids,nakijinamines, from a sponge Suberites sp.

The structures of seven new secondary metabolites isolated from an Okinawan marine sponge Suberites sp., nakijinamines A (1), B (2), and F–I (3–6) and 6-bromoconicamin (7), have been elucidated on the basis of spectroscopic analysis, chemical conversion, and conformational analysis. These analyses disclosed that 1–6 were heteroaromatic alkaloids having the hybrid structures of an aaptamine-type alkaloid and an indole alkaloid, while 7 was a bromoindole alkaloid. Nakijinamine I (6) is the first example of an aaptamine-type alkaloid possessing a 1,4-dioxane ring. Antimicrobial activities of 1–7 were evaluated.     

Fused-s-triazino heterocycles. XII. 13H-4,6,7,8,13a, 13c-hexaazabenzo-[de]naphthacene,a new ring system

The synthesis of the titled compound is described using 5-(2-carboxyanilino)-2-methyl-1,3-4,6,9b-pentaaza-phenalene as starting material.     

Oxidative coupling of 4a,9-diaza-1,2,4a,9a-tetrahydrofluorenes. 1. Synthesis of mononuclear heterocyclic quinonediimines

Oxidative coupling of 4a,9-diaza-1,2,4a,9a-tetrahydro-9H-fluorene with primary amines and ammonia in the presence of MnO₂ gives the corresponding 6-aryl (or alkyl)imino-4a,9-diaza-1,2,4a,9a-tetrahydro-6H-fluorenes. Coupling with thiourea under these conditions affords 6-cyanoimino-4a,9-diaza-1,2,4a,9a-tetrahydro-6H-fluorenes.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, pp. 1500–1504, November, 1989.     

Zur Bestimmung des Albumingehaltes in Serum, Urin u. a.

Ohne Zusammenfassung     

Eine Bestimmung von Cu-Spuren in Ni, Cd, Zn, Co, Mn, Al und Erdalkalien mittels p.a. IDE-Harz

Ohne Zusammenfassung