3,4—亚甲二氧基苯甲酸锡酯的合成及表征

３，４－亚甲二氧基苯甲酸及其取代物与三苯基氢氧化锡或二丁基化锡反应合成了５个锡酯，通过元素分析，ＩＲ和＾１ＨＮＭＲ对其进行了表征。     

1─芳氧基乙酰基─4─苯甲酰氨基硫脲衍生物的合成及其生物活性研究

１─芳氧基乙酰基─４─苯甲酰氨基硫脲衍生物的合成及其生物活性研究魏太保，陈继畴（西北师范大学化学系，兰州，７３００７０）杨素铀，王秀春（西北师范大学生物系，兰州，７３００７０）关键词：１—芳氧基乙酰基—４—苯甲酰基氨基硫脲，相转移催化，合成，生物活性...     

The Reaction of 4-Formylsydnone with Nitroalkanes

Under various basic solutions and reaction durations, 3-substituted 4-formyIsydnones and nitroalkanes containing α-active hydrogen (e.g. nitromethane and nitroethane) are converted to β-nitroalcohols, nitroalkenes and dinitroalkanes. β-Nitroalcohols are obtained only by electrochemical reaction on an electrogenerated base (EGB). The mechanism of overall reaction steps in particular is discussed.     

新显色剂二溴硝基苯基重氮氨基偶氮苯的合成及与镉的显色反应的研究

作者合成了新显色剂2,6-二溴-4-硝基苯基重氮氨基偶氮苯(DBNDAA)。在pH8.5的硼砂-盐酸缓冲介质中,在Tween 80-SDBS存在下,该试剂与镉(Ⅱ)生成络合比为3:1的红色络合物,λ_(max)=500nm,ε_(500)=1.52×10~5L·mol~(-1)·cm~(-1)。镉量在0～28μg/25ml范围内遵守比耳定律。并测定了试剂的表观离解常数和络合物的表观不稳定常数。方法有良好的选择性。用该试剂测定了铝合金标样、环境水样及废水中的痕量镉,结果满意。     

Reaktionen vonN-Sulfinylverbindungen mit dem 1,2,4-Trithia-3,5-diborolan-Ringsystem und Substitutionsreaktionen am 1,2,4-Trithia-3,5-diborolan und 1,2-Dithia-4-aza-3,5-diborolidin

The reaction of trimethylsilyl- and pentafluorophenyl-N-sulfinylamine respectively with 3,5-dihalogeno-1,2,4-trithia-3,5-diborolanes yields the 1,2-dithia-4-aza-3,5-diborolidines1-3.Tert-butyl-N-sulfinylamine and 3,5-dimethyl-1,2,4-trithia-3,5-diborolane react analogous. OtherN-sulfinylamines however split the disulfane bridge in 3,5-dimethyl-1,2,4-trithia-3,5-diborolane and the 1,4-dithia-2-aza-3,5-diborolidines5A-7(A) are formed. Besides of boroxines, cyclo-2,4,6-trimethyl-1,3-dioxa-5-aza-2,4,6-triboranes and cyclo-2,4,6-trimethyl-1-oxa-3,5-diaza-2,4,6-triboranes are formed as byproducts,8–10 have been isolated. In 1,2,4-trithia-3,5-diborolanes and 1,2-dithia-4-aza-3,5-diborolidines the bromo-atoms can be substituted by alkyl (13, 14), by amino (15–20) and by isothiocyanato groups. The compounds were characterised analytically and spectroscopically (MS; NMR:¹H,¹¹B,¹⁹F,²⁹Si; IR).

     

Trigonal-planare CuX3-Gruppen in Cu2Mo6X14, X = Cl,Br, I

Trigonal Planar CuX₃-Groups in Cu₂Mo₆X₁₄, X = Cl, Br, I Cu₂Mo₆Cl₁₄ (I), Cu₂Mo₆Br₁₄ (II) and Cu₂Mo₆I₁₄ (III) were synthesized by thermal treatment of corresponding mixtures of copper(I) and molybdenum(II) halides. The crystal structures were determined by single crystal X-ray analyses. I and II show isotypism, cubic, Pn3 (no. 201, sec. setting), Z = 4, I: a = 12.772(3) Å, II: a = 13.350(2) Å. III shows a new structural type, orthorhombic, Pbca (No. 61), Z = 4, a = 16.058(3) Å, b = 10.643(2) Å, c = 16.963(3) Å. Trigonal planar CuX₃ units were found in I? III. Structural behaviour relations are discussed, especially with regard to ionic conductivity.     

Synthese und Strukturuntersuchungen von Ba2H[α-FeO4W12O36] · 26 H2O

Synthesis and Structure Studies of Ba₂H[α-FeO₄W₁₂O₃₆] · 26 H₂O The heteropolyanion compound Ba₂H[α-FeO₄W₁₂O₃₆] · 26 H₂O (I) crystallizes in the tetragonal space group P4 n2 with the lattice parameters a = 12.398(6), c = 18.721(6) Å; Z = 2; D_x = 4.128 g · cm^?3. The structure was solved on a twinned crystal from 1029 observed reflections and refined to an index R of 7.6%. The calculations were done by means of a modified ORFLS-programme by Eitel and Bärnighausen. The heteropolyanion [α-FeO₄W₁₂O₃₆]^5? has the well known α-Keggin structure. The average distance of the four central oxygen atoms to the Fe^III position (0, 0, 0) is 1.84 Å. The angles ? O? Fe? O are 112.3° (4X) and 103.9 (2X), respectively, which leads to an disphenoidal distortion of the FeO₄ tetrahedron. The powder and single crystal ESR spectra of I show the anisotropy of the Fe^III fine structure transition 1/2 ? ?1/2. The Mößbauer spectra confirm the tetragonal distortion of the central FeO₄ tetrahedron (quadrupole splitting Δ ≈ 0.50 mm · s^?1).     

The research on the high quality TiO2, MoO3-doped WO3 electrochromic film

The high quality TiO2, MoO3-doped WO3 electrochromic film was prepared by the sol–gel method for the first time. The sol, which has hydrogen peroxide (H2O2) and oxalic acid (H2C2O4), was very stable at room temperature and quite suitable for the deposition of films. The WO3 electrochromic film prepared from this doped sol had excellent performance, such as short response time, no cracks, good adhesion to the substrate, high coloring efficiency and longevity of service.     

Reactivity of N-alkyl derivatives of hydroxylamine in decomposition of 4-nitrophenyl diethylphosphonate in water and in cetyltrimethylammonium bromide micelles

Neutral forms of hydroxylamine, N-methylhydroxylamine, and N,N-dimethylhydroxylamine are typical α-nucleophiles in water. In comparison with aryl anions of similar basicity their rate of reaction in the decomposition of 4-nitrophenyl diethylphosphonate is increased by about 10² times. Decomposition of the substrate is accelerated in cetyltrimethylammonium bromide micelles (about 4 to 30 fold). Hydroxylamine and its N-alkyl derivatives are the most effective low basicity nucleophiles. The sole factor responsible for the micellar effects is the concentration of the reagent in the surfactant micelles. __________ Translated from Teoreticheskaya i éksperimental’naya Khimiya, Vol. 43, No. 4, pp. 231–236, July–August, 2007.     

基于氮化碳复合材料磁性固相萃取结合高效液相色谱法测定尿液中3种羟基多环芳烃

建立了测定尿液中3种羟基多环芳烃的氮化碳复合材料磁性固相萃取结合高效液相色谱-荧光检测法。所构筑的磁性氮化碳材料，经扫描电子显微镜、X射线衍射仪、振动样品磁强计和比表面积分析仪表征后，用于尿液中3种羟基多环芳烃的富集净化。考察了吸附剂用量、吸附时间、洗脱溶液和洗脱体积（单次洗脱体积×洗脱次数）对萃取效率的影响。结合高效液相色谱-荧光分析，在0.25~250 μg/L范围内线性关系良好（相关系数r=0.999），3种羟基多环芳烃的检出限和定量限分别为0.08和0.25 μg/L，回收率为90.1%~102%，日内和日间精密度分别为1.5%~7.7%和2.2%~8.7%。该本方法简单、快速、高效，可用于尿液中羟基多环芳烃的分析。