Synthesis ofS-(+)-hydroprene

A novel path toS-(+)-hydroprene (1) starting from the technical gradeS-(+)-dihydromyrcene (2, e.e. 50%) is proposed. The latter was selectively transformed intoS-3,7-dimethyloctanal (5) in three steps including hydroalumination. The reactions of5 with allyl- or methallylmagnesium chloride followed, respectively, either by oxygenation in the presence of PdCl₂/CuCl or by ozonolysis, affordS,E-6,10-dimethyl-3-undecen-2-one (7) which was treated with ethoxyethynylmagnesium bromide to give the title juvenile hormone analogue in 23% overall yield.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No 1, pp. 110–112, January, 1993.     

Investigations of benzimidazole derivatives

3-(1-Methyl-2-benzimidazolyl)acrylic acid was obtained by the reaction of 1,2-dimethylbenzimidazole with chloral and subsequent hydrolysis of the condensation product. The hydrochloride of the chloride of this acid and its esters and amides were synthesized. The methyl and ethyl esters of the acid were synthesized by the Wittig reaction. The IR and UV spectra of the compounds obtained are presented.See [9] for Communication XXIV.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, pp. 1566–1568, November, 1970.     

Synthesis and Structure of the New Ammonium Indium Phosphate (NH4)In(OH)PO4

A new ammonium indium phosphate (NH₄)In(OH)PO₄ was prepared by hydrothermal reaction in the In₂O₃-NH₄H₂PO₄-NH₃/OH system (T=200°C, autogenous pressure, 7 days). The formula (NH₄)In(OH)PO₄ was determined on the basis of chemical and thermal analysis (TG/DSC), X-ray powder diffraction and IR-spectroscopy. (NH₄)In(OH)PO₄ crystallizes in the tetragonal system with space group P4₃2₁2 (No. 96); a=9.4232(1) Å, c=11.1766(1) Å, V=992.45(2) ų; Z=8. The crystal structure was refined by the Rietveld method (R_w=6.35%, R_p=5.10%). The second-harmonic generation study confirmed that structure of (NH₄)In(OH)PO₄ does not have a center of symmetry. The cis-InO₄(OH)₂ octahedra form helical chains, parallel to the c-axis. The In-O-In bonds are nearly equidistant. The chains are interconnected by phosphate tetrahedra and create tunnels containing the NH₄⁺ ions along the c-axis. (NH₄)In(OH)PO₄ is isostructural with RbIn(OH)PO₄.     

Ion-exchange properties of silica gel with covalently bonded histidine

The ion-exchange and acid-base properties of Silasorb 600 (10 μm) with immobilized histidine (His-SiO₂) were investigated. The acid-base properties of the sorbent were estimated from the dependence sof the retention of organic acids and bases on the eluent pH. The effect of various organic modifiers (benzoic, citric, oxalic, and sulfuric acids) and the eluent pH on the retention of inorganic ions was studied. It was shown that His-SiO₂ exhibits anion-exchange properties in acidic and weakly acidic media at pH < 5.7. Eight anions were separated under optimal conditions on a 150 × 4.6-mm column in 21 min using a 5 mM oxialic acid solution as an eluent.     

Quantitative estimation of the α-effect in the reactions yielding phosphorus-containing thiosemicarbazides

The α-effect in the reactions of O,O-diaryl phosphorohydrazidothioates with phenyl isothiocyanate in benzene at 25°C was quantitatively evaluated from the kinetic data. The probable reaction mechanism was suggested, and the causes of the α-effect in these reactions are discussed. An approximate linear correlation is observed between the α-effect in the reactions of O,O-diaryl phosphorohydrazidothioates with phenyl isothiocyanate, basicity constants of the hydrazides, and σ^p constants of the substituents at the P atom. The value of the α-effect is largely determined by the structure of the transition state.     

Isoscalar factors for tetragonal,orthorhombic, monoclinic and triclinic shubnikov point groups

The relations between isoscalar factors for corepresentations of antiunitary magnetic point groups are discussed in the case of associated corepresentations. The tables of the isoscalar factors for the single- and double-valued corepresentations of all tetragonal, orthorhombic, monoclinic, and triclinic Shubnikov point groups are given. Some peculiarities of the calculation method of the isoscalar factors for corepresentations are considered.     

Synthesis and properties of N-methylmorpholinium 4aryl-6-methyl-5-phenylcarbamoyl-3cyano-1,4dihydropyridine-2-thiolates. Molecular and crystalline structure of 2allylthio-6-methyl-5-phenylcarbamoyl-4-(2chlorophenyl)-3-cyano-1,4-dihydropyridine

By the condensation of an aromatic aldehyde, the anilide of acetoacetic acid, cyanothioacetamide, and Nmethylmorpholine, substituted N-methylmorpholinium 1,4-dihydropyridine-2-thiolates have been synthesized and subsequently used in the synthesis of the corresponding thiones, 2-alkylthiopyridines, thieno[2, 3b]pyridines, and disulfides. X-ray diffraction has been used to establish the structure of 2-allylthio-6-methyl-5phenylcarbamoyl-4-(2-chlorophenyl)-3-cyano-1, 4-dihydropyridine.T. G. Shevchenko Lugansk State Pedagogical Institute, Lugansk 348011. A. N. Nesmeyanov Institute of Heteroorganic Compounds, Russian Academy of Sciences, Moscow 117813. N. D. Zelinskii Institute of Organic Chemistry, Russian Academy of Sciences, Moscow 117913. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1243–1251, September, 1996. Original article submitted May 13, 1996.     

Effect of modified fibre glass on the structure and thermophysical properties of pentaplast(pentane)

The results of experimental investigations of the effects of ground fibre glass on the structural parameters and thermophysical characteristics of pentaplast(pentane) were assessed.The degree of crystallinity, thermal conductivity, specific heat and density of pentaplast containing various amounts of modified fibre glass were determined experimentally.The results obtained are discussed in terms of modern theories of the effects of fillers on the properties and structures of polymers.

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Zusammenfassung Es werden die Ergebnisse der experimentellen Untersuchungen des Einfl usses von gemahlenem Fiberglas auf die Strukturparameter und thermophysikalischen Eigenschaften von Pentaplast (Pentan) gewertet.Der Kristallinitätsgrad, das Wärmeleitvermögen, die spezifische Wärme und die Dichte von Pentaplast mit verschiedenem Gehalt an modifiziertem Fiberglas wurde experimentell ermittelt.Die erhaltenen Ergebnisse wurden hinsichtlich moderner Theorien über den Einfluß von Streckmitteln auf die Eigenschaften und die Struktur von Polymeren diskutiert.

     

13C-NMR. Spectroscopy of naturally occurring substances. XXXII. Vincaleucoblastine and related alkaloids.

The total assignment of the ¹³C-shifts of the complex Vinica rosea L. alkaloids vincaleucoblastine, leurosidine and leurosine and of a synthetic isomer of the latter is presented. The structure of leurosidine is corrected and a tentative structure for the acid-catalyzed product of isomerization of leurosine is proposed.     

Chemistry of heteroanalogs of isoflavones. 16. Benzthiazole analogs of isoflavones

The reaction of a-(2-benzthiazolyl)-2, 4-dihydroxy-5-alkylacetophenones with anhydrides and chlorides of carboxylic acids yielded 3-(2-benzthiazolyl)chromones with electron-acceptor and electron-donor substituents, as well as chromones unsubstituted in the 2 -position. Their acylation, alkylation, and aminoacylation reactions and their interaction with electrophilic and nucleophilic reagents were studied.Taras Shevchenko Kiev University, Kiev 252017. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 464–471, April, 1994. Original article submitted March 5, 1994.