Solid-phase synthesis of amidines by the reduction of amidoximes

Amidines can be prepared on a solid support by reducing polymer-bound amidoximes with SnCl₂·2H₂O. The method has proved to be straightforward and highly efficient. Amidoximes attached to the solid support are readily available by treating resin-bound nitriles with hydroxylamine.     

Molecular structure of potassium [N,N′-bis(salicylideneamino)nitroguanidonate-N,N′,-O,O′]nickel(ii), the product of condensation of (salicylideneamino)nitroguanidine with salicylaldehyde on a Ni2+ ion template

The crystal structure of the product of the condensation of (salicylideneamino)nitroguanidine with salicylaldehyde on a Ni²⁺ ion template, K[Ni(C₁₅H₁₀N₅O₄)] · DMF, has been studied. It was established that a planar Ni complex, consisting of isolated [NiL]^– anions and solvated [K⁺ · DMF] cations, is formed. The negative charge of the anion is localized mainly on the O atoms of the nitro group. The nitroguanidine fragment of the ligand occurs in the tautomeric form, which was not reported previously.Deceased in 1995Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 2273–2277, September, 1996.     

溶胶-凝胶法制备高取向Bi4Ti3O12/SrTiO3(100)薄膜

Bi4Ti3O12具有良好的铁电、电光等性能山、特别是Bi4Ti3O12薄膜很适合作永久性存储材料，也可用于电光器件问．在微电子学、光电子学、集成光学、集成铁电学等领域均有广泛开发和应用前景，国外已用溅射法、激光沉积法制备出c轴取向Bi。Ti3Ol。薄膜【’，＼山东大学用MOCVD法制     

Ar原子电离能谱和Ar3p电子动量谱研究

电子动量谱学（ElectronMomentumSPectroscoP则是近．二十年来发展起来的一种新兴的探测原子、分子和固体结构的手段，它不仅能够获得轨道结合能的信息，而且能够能壳分辨地得到轨道电子的动量分布（即动量表象中的波函数模方）；同时它还是研究电子关联的最有效的实验手段．其     

Molecular Structure of 1,3,5-Tris (Trimethylstannyl) Benzene: An Electron Diffraction Study

The molecular structure of 1,3,5-tris (trimethylstannyl) benzene has been determined by gas-phase electron diffraction. The C — C bond length is in good agreement with that in benzene. In agreement with the somewhat electron-releasing character of the substituents, the endocyclic bond angles at the substituents are somewhat smaller than 120°. The mean value of Sn — C bond lengths is greater than that in tetraphenyltin and tetramethyltin. The SnMe₃ groups appear freely rotating around the C_aryl — Sn bonds. The following bond lengths (r _g) and bond angles were determined: (Sn — C)_mean 2.150 ± 0.007 Å, C — C 1.399 ± 0.005 Å, (C — H)_mean 1.105 ± 0.006 Å, < C — C(Sn) — C 117.7 ± 1.7º, < C_aryl — Sn — C_methyl 106.7 ± 0.7º < Sn — C — H 111.5 ± 0.9º.     

Voltammetric Detection of Free Sulfhydryl Compounds in Food Flours

Cyclic voltammetry has been applied to the rapid measurement of free SH‐compounds in food flours samples. The protocol is based on the electrochemical adaptation of the Ellman's test, where the DTNB reacts with SH‐compounds present in food flour extracts, resulting in the equimolar production of the electroactive compound TNBA which, in turns, reacts with phenylendiamine. The reaction is found to provide an analytical signal from which to quantify indirectly free sulfhydryl compounds in flours extracts.     

Synthesis and anticonvulsant activity of new fluorinated N-phenyl- and N-benzyl-2-azaspiro[4.4]nonane- and [4.5]decane-1,3-dione derivatives: Part III

A series of N-phenyl- and N-benzyl-2-azaspiro[4.4]nonane- and [4.5]decane-1,3-diones containing a fluoro or trifluoromethyl substituents at the aryl ring was synthesized and tested for their anticonvulsant activity in the maximal electroshock (MES) and subcutaneous metrazole (sc.Met) tests. Among them, the most active were N-benzyl derivatives with fluoro and trifluoromethyl substituents especially at position-2 of the aryl moiety. The introduction of the phenyl ring at the imide nitrogen atom resulted in less active compounds. The results obtained showed that incorporation of fluoro or trifluoromethyl substituents increased the anticonvulsant activity in comparison to respective chloro, methoxy or methyl analogues. Crystallographically obtained conformation for one active and two inactive derivatives with trifluoromethyl substituents at position-2 or -3 of phenyl ring were initially used for molecular electrostatic potentials (MEP) calculation. The MEP distribution at carbonyl oxygen atoms was different for active and inactive molecules.     

The effect of (natural) polyols on the initial colour of heavy metal- and zinc-free poly(vinyl chloride)

The propensity of (natural) polyols dispersed in heavy metal- and zinc-free PVC sheets to improve the initial colour, e.g. the colour during the first minutes of exposure to high processing temperatures (short-term stability), has been investigated. It is shown using W(Lab) values that the initial colour improves upon addition of polyols containing primary hydroxyl groups. The polyols act as HCl scavengers, presumably via an acid-catalysed S_N2 substitution of the primary hydroxyl groups by chloride ions. In contrast, polyols with only secondary or tertiary hydroxyl groups accelerate the thermal degradation of PVC. Notwithstanding, the efficacy of the (natural) polyols containing primary hydroxyl groups will be reduced if the polyol is susceptible to competitive acid-catalysed intramolecular cyclodehydration reactions under the processing conditions. This is substantiated by a comparison of the behaviour of mannitol and 3,4-di-O-methyl-d-mannitol. The methylated derivative, which is less prone to undergo intramolecular cyclodehydration, improves the initial colour of heavy metal- and zinc-free PVC sheets more significantly than mannitol itself.     

Flavonoids of <Emphasis Type="Italic">Scutellaria immaculata</Emphasis> Roots

(±)-5,2′-Dihydroxy-6,7,6′-trimethoxyflavanone, (-)-5,2′-dihydroxy-6,7,8,6′-tetramethoxyflavanone, chrysin, wogonin, apigenin, isoscutellarein, scutellarein, cosmosiin, and the new flavonoid wogonin-7-O-β-D-glucopyranoside, the structure of which was established using chemical transformations and spectral data, were isolated from Scutellaria immaculata roots.__________Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 26–28, January–February, 2005.     

Highly tilted antiferroelectric (R) enantiomers useful for the formulation of eutectic mixtures

ABSTRACT

Novel chiral three-ring (R) enantiomers were synthesised using optically active (R)-(?)-2-octanol. Properties, such as the sequence of phases, the transition temperatures and enthalpies, were tested by a polarising optical microscope and differential scanning calorimeter. An antiferroelectric smectic phase (SmC_A*) with a direct transition from the antiferroelectric to the isotropic phase (SmC_A*-Iso) was observed for three esters with an achiral C₃F₇CH₂O(CH₂)₃O– terminal chain. Bi- and multicomponent mixtures with a broad temperature range of the antiferroelectric phase and good electro-optical properties were formulated. Helical pitch of pure esters and mixtures was measured by spectrophotometry method.