Analysis of tetrapyrrolic pigments and derivatives in sediments by high performance liquid chromatography/atmospheric pressure chemical ionization mass spectrometry

A new application is described of the on-line high-performance liquid chromatography/positive and negative ion atmospheric pressure chemical ionization mass spectrometry (APCI(+/–)-MS) to the identification of tetrapyrrolic compounds in sediment samples containing complex mixtures of natural pigments and their diagenetic products. The method relies on the production of radical anions in order to determine the molecular masses of the molecules which yield abundant fragment ions when analyzed in the positive mode. This approach allows to verify the occurrence of coeluting components by examining their negative ion spectra and to complete their identification on the basis of their fragment ions produced in the positive ion spectra. Received: 24 September 1998 / Revised: 23 December 1998 / Accepted: 29 December 1998     

Amino acid derivatives of 2-R-7-hydroxy-3′,4′-ethylenedioxyisoflavones

A number of 7-O-aminoacyl derivatives of isoflavones have been obtained by the interaction of 2-R-7-hydroxy-3,4-ethylenedioxyisoflavones with the symmetrical anhydrides of N-protected amino acids.Kiev Tara Shevshenko University, Ukraine, 252033, Kiev, Ul. Vladimirskaya, 64, tel./fax 225-12-73. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 334–338, May–June, 1999.     

咪唑钴啉酯的合成及钴—氮键稳定性的研究

合成了维生素B_(12)(VB_(12))模型分子—单腈N-甲基3-咪唑基钴啉酯高氯酸盐8。通过8在不同pH缓冲溶液中的UV-Vis谱,计算了Co—N键的平衡常数,独立配位体N-甲基咪唑与咕啉环中心钴原子配位键的键强与自身键连配位体的配位键强要弱。     

Catalysis by titanium (IV) ions of reactions forming chlorohydrins from olefins

A study was made of reactions forming chlorohydrins from cyclohexane and other olefins acted upon by H₂O₂ and HCl or H₂O₂ and TiCl₄ in alcoholic solutions. The catalyzing action of titanium (1V) was established, and possible reaction mechanisms are discussed.L. V. Pisarzhevskii Institute of Physical Chemistry, National Academy of Sciences of Ukraine, 31 Prosp. Nauki, 252039, Kiev, Ukraine. Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 32, No. 5, pp. 295—299, September–October, 1996. Original article submitted February 9, 1996.     

Tantalum(v) oxoalkoxides. Synthesis and structure

Anodic oxidation of tantalum in isopropyl alcohol or prolonged reflux of an alcohol solution of Ta(OPrⁱ)₅ afford crystalline oxoisopropoxide Ta₂O(OPrⁱ)₈ · PrⁱOH (1). In its molecule, two octahedra about Ta atoms are linkedvia the shared edge [(OPrⁱ)O]. Compound1 is the first example of oxoalkoxide containing such a small number of metal atoms. Unlike the known polynuclear molecules M _n O _m (OR) _p , oxoalkoxide1 is stable in solutions; on transition to the gas phase, this compound is desolvated to form a very stable molecule Ta₂O(OPrⁱ)₈ (apparently, consisting of two octahedra with a shared edge). According to the data of mass spectrometry, analogous molecules exist in the gas phase over Ta(OAlk)₅ (Alk = Me, Et, Prⁱ, or Bu¹¹). When compound1 is heated invacuo (10^–2–10^–3 Torr), Ta(OPrⁱ)₅ is sublimated. Crystals of Ta₇O₉(OPrⁱ)₁₇ (2) were formed upon prolonged storage of solutions of1 in PrⁱOH. Heptanuclear molecule2 consists of two [Ta₄] tetrahedra with a shared vertex. These tetrahedra are additionally linked togethervia one ₃-oxo and two ₂-OPrⁱ groups. Complex2 is a representative of heptameric oxoalkoxides of a new structural type.Deceased in I995.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 125–131, January, 1996.     

Polyaniline films doped with zinc salts and their properties

It has been found that thin polyaniline films doped with several zinc salts in solutions at pH 5.5 become electroconductive and electroactive in neutral aqueous electrolytes. The shape of the voltammetric characteristics depends on the initial state of the film. The effect of secondary doping withm-cresol is observed for polyaniline complexes with zinc salt of camphorsulfonic acid.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1450–1452, June, 1996.     

Syntheses based on dimethylpyrazoles. 9. Synthesis and spectral peculiarities of isomeric pyrazolo[3′,4′-5,6]- and-[5′,4′-5,6]-pyrimido[1,2-b]benzo[d,e]isoquinoline-4,12-diones

2-Methyl-2,4,12,13H-pyrazolo[3,4-5,6]pyrimido[1,2-b]benzo[d,e]isoquinoline-4,12-dione and its 8-nitro- and 8-amino-substituted derivatives were obtained starting from 4-amino-3-carbamoyl-1-methylpyrazole and naphthalic and 4-nitronaphthalic anhydrides. The spectral properties of the synthesized compounds were studied.See [1] for Communication 8.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, pp. 237–241, February, 1990.     

Catalytic properties of V?Sb?O systems in acrolein oxidation

Catalytic properties of V-Sb-O systems in acrolein oxidation have been studied. It has been established that the changes in the activity and selectivity of the catalysts are due to the phase and chemical properties of the system.

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Oxidation of hexadec-11Z-en-1-ol by Cr(VI) reagents on polymeric supports

A method is proposed for the oxidation of hexadec-11Z-en-1-ol to hexadec-11Z-enal by Cr(VI) reagents on polymeric supports.A. S. Sadykov Institute of Bioorganic Chemistry, Uzbek Academy of Sciences, Tashkent. V. I. Lenin Tashkent State University. Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 252–255, March–April, 1990.     

Preparation of rare metallic actinides (248Cm,249Bk,249Cf) and investigation of their crystal structure

²⁴⁸Cm and²⁴⁹Bk metals were prepared by thermal reduction of their oxides with thorium and metallic²⁴⁹Cf with metallic lanthanum. These rare actinide samples of 1.0 mg in mass were thin layers on a flat substrate and were investigated by X-ray technique. Dhcp lattice parameters of -Cm, -Bk and -Cf as main phases in X-ray diagrams are presented. The effect of impurities on the -Cm lattice parameters is shown. Fcc lattices for the high temperature form of Cm metal (-Cm) with a=0.4933 nm, and of Cm and Bk monoxides (a=0.502–0.504 nm and a=0.5002 nm, respectively) have been observed. Thermal expansion coefficients for -Cm and -Bk at 80–300 K were calculated. Identification problems of fcc lattices and oxidation features of metals prepared are discussed.