Synthesis of s-triazolocycloalkyl-, s-triazolobenzocycloalkyl-, and s-triazolocycloalkylhydrothiadiazines

The reaction of cyclic-α-haloketones with 5-subslituted-4-amino-4H-1,2,4-triazole-3-lhiols gave s-triãzolocycloalkylhydrothiadiazines and s-triazolobenzocycloalkylthiadiazines. Reduetion of the 5,5a-imine bond of the s-triazoloeycloalkylthiadiazines gave s-triazolocycloalkylhydrothia-diazines.     

Kinetic study and analytical application of the iodate-hypophosphite reaction in strongly acidic solutions

The iodate—hypophosphite reaction in strongly acidic solutions was studied spectrophotometrically. Reaction rate constants and the activation energy of the reaction are reported. A method for determining hypophosphite on the basis of this reaction is described. Hypophosphite in the range 0.06–4 mg (10^-3–6·10^-2 M) can be determined with a relative error and relative standard deviation of 2—3%.     

1H-NMR-spektroskopische konformationsanalyse von halogenierten thymidinabkömmlingen: I. konformation von thymidin, 3',5'-didesoxy-3'-chlor-5'-fluor-thymidin und 3', 5'-didesoxy-3',5'-difluor-thymidin

An improved method is given for determining the conformation of furanoid nucleosides by ¹H-NMR-spectra analysis using halogen-substituted thymidines as examples. The state of the three equilibria - ring-puckering, rotation about the C₄-C₅- bond and about the glycosidic bond - are influenced by the halogen substituents. Compared with thymidine the 3'-chlorine substituent shifts the furanose conformation to conformers, where the 3'-chlorine substituent is equatorial. The 5'-fluorine substituent increases the contribution of the G-G-rotamer and the ratio of syn-conformation. The relationships between the conformers in the pseudo-rotatory cycle and the population of the C_4'-C_5' rotamers are discussed.     

Synthesis and some properties of acrylic and methacrylic derivatives of chlorophos and its analogs

Conclusions The reaction of chlorophos and its analogs with the acid chlorides of the acrylic, methacrylic and-fluoroacrylic acids gave some new unsaturated compounds that possess fungicidal action.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 4, pp. 883–886, April, 1973.     

Über halogen- und stickstoffhaltige Derivate aliphatischer Carbonsäuren, 10. Mitt. (Über Reaktionen mit Aluminiumalkylen, 13. Mitt.): Über die Reduktion von tertiären α-Nitrocarbonsäureestern mit LiAlH4, Diisobutylaluminiumhydrid und Diäthylaluminiumhydrid

Zusammenfassung Die Reduktion tertiärer -Nitroester mit LiAlH₄ verläuft anomal. Infolge Abspaltung der Carboxylgruppe sind Aminoalkane Hauptprodukte dieser Reduktion. Daneben entstehen in geringer Menge unter Erhaltung des Kohlenstoffgerüstes -Hydroxylaminoalkohole. Diese Reaktion wird mit der Reduktion von sekundären -Nitroestern und von -Oximinoestern verglichen.Mit Dialkylaluminiumhydriden erleiden die tertiären Nitroester ebenfalls in der Hauptsache Reduktion unter C-C-Spaltung zu Aminoalkanen. Eine Nebenreaktion führt jedoch über die Stufe der Hydroxylaminoalkohole hinaus zu Aminoalkoholen. Außerdem tritt alkylierung am Stickstoffatom zu Alkylaminoalkanen bzw.-alkoholen auf.

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Halogen and nitrogen containing derivatives of aliphatic carboxylic acids, X (reactions with aluminium alkyls, XIII): Reduction of tertiary -nitro carboxylic acid esters with LiAlH₄, diisobutyl aluminium hydride, and diethyl aluminium hydride

The reduction of tertiary -nitro esters with LiAlH₄ proceeds anomalously. As a result of a decarboxylation amino alkanes are the main products of this reductions. Besides -hydroxylamino alcohols are obtained in small amounts by conservation of the carbon skeleton. This reaction is compared with the reduction of secondary -nitro esters and of -oximino esters.Tertiary -nitro esters are reduced by dialkyl aluminium hydrides to amino alkanes under cleavage of the C-C-bond. In a side-reaction one obtains amino alcohols via the stage of hydroxylamino alcohols. Besides the nitrogen atom is alkylated leading to alkylamino alkanes respectively alkohols.

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9. Mitt.:H. Reinheckel, Mh. Chem.99, 2215 (1968).

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12. Mitt.:H. Reinheckel undR. Gensike, J. Organometal. Chem.13, 45 (1968).     

A Sensitive HPTLC Method for Estimation of Amentoflavone,a Bioactive Principle from Biophytum sensitivum (Linn.) DC. and Putranjiva roxburghii Wall.

JPC – Journal of Planar Chromatography – Modern TLC - A sensitive high-performance thin-layer chromatographic (HPTLC) method has been developed for estimation of amentoflavone, an...     

Reaction of 5-haloanthra[1,9-cd]-6-isoxazolones with aziridine

The reaction of 5-haloanthra[1,9-cd]-6-isoxazolones with aziridine gave 5-aziri-dinoanthra[1,9-cd]-6-isoxazolones. The latter, upon reaction with acids, undergo cleavage of the aziridine ring.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 7, pp. 885–888, July, 1984.     

Synthesis and chiral-optical properties of some benzolactams

Five- and seven-membered benzolactarns — (–)-S-2, 3-dimethyl-2, 3-dihydroisoindolone and (+)-S-5-methyl-2, 3, 4, 5-tetrahydrobenz[c]azepin-1-one — were synthesized. A study of their chiral-optical properties and comparison with the previously studied six-membered lactam (–)-S-4-methyl-3, 4-dihydroisoquinol-1-one showed that their circular dichroism spectra are similar: The spectra contain dichroic absorption bands due to ^* transitions in the aromatic chromophore (270 and 220 nm) and a band of charge transfer in the benzamide chromophore at 240–250 nm. The magnitude of the Cotton effect due to the charge-transfer band increases as the lactam ring becomes larger (five-membered < six-membered < sevenmembered benzolactam). The change in the magnitude of the Cotton effect is explained by the development of a strictly dissymetric chromophore.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 656–662, May, 1978.     

The application of linear discriminant analysis in the diagnosis of thyroid diseases

The effectiveness of five in-vitro laboratory tests for differentiation between three thyroid functional states (EU, HYPO and HYPER thyroidism) has been determined by using statistical linear discriminant analysis. The optimal linear combination of laboratory tests obtained by means of linear discriminant analysis results in a better use of the information present in each test, so that the possible redundancy of tests can be assessed. In this context, some feature selection criteria were evaluated. It is shown that in this application only two laboratory tests are necessary to obtain a sufficiently high diagnostic effectiveness when linear discriminant analysis is applied.     

First-principles calculations of K-edge X-ray absorption near edge spectra of some transition metal dimers

Theoretical X-ray absorption near-edge spectra have been evaluated for different bond lengths of Mn₂, Co₂ and Ni₂ using a modified Xα scattered-wave procedure.