新显色剂四(邻氯对磺酸基苯基)卟啉导数分光光度法同时测定镉和铅的研究

在pH 10.7,有溴化十六烷基二甲基乙酸铵存在,咪唑催化新显色剂四(邻氯对磺酸基苯基)卟啉与镉和铅反应生成三元胶束络合物,最大吸收波长分别为437和470nm,其表观摩尔吸光系数相应为5.6×10~5和2.0×10~5。用二阶导数分光光度法同时测定镉和铅,结果满意。     

四(4-硝基苯基)卟啉和四(4-氨基苯基)卟啉的合成

四（４氨基苯基）卟啉（ＴＡＰＰ）是含有４个反应活性基团的卟啉衍生物,可在模拟某些生物过程或氧化还原反应的树枝状或簇状分子中作为富电子中心,也可直接用来制备光电器件或作为光电功能聚合物的功能单体和交联剂,因此,ＴＡＰＰ的合成研究具有重要意义［１］．...     

Selective Decarboxylation: A Facile Synthesis of 3-Pyridinecarboxylic Acid Derivative

A convenient synthesis of 5-trifluoromethyl-3-pyridinecarboxylic acid was developed, involving palladium-catalyzed carbonylation, hydrolysis, and decarboxylation. This novel route features inexpensive starting material and easy operations.     

Cyclophane bis(sulfoxides) a thermal analysis study

A thermogravimetry study of a series of cyclophane bis(sulfoxides) (1–6) has shown that thermal decomposition of these compounds occurs in two stages with a stepwise loss of the sulfoxide groups at well defined decomposition temperatures. The stepwise thermal cleavage has been rationalized in terms of the stereochemistry of the sulfoxide groups and the strain associated with the resultant elimination products.

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Zusammenfassung Eine thermogravimetrische Studie einer Reihe von Cyclophan-bis(sulphoxiden) (1–6) zeigte, dass die thermische Zersetzung dieser Verbindungen in zwei Stufen unter stufenweisem Verlust der Sulphoxidgruppen bei gut definierten Zersetzungstemperaturen vor sich geht. Die stufenweise thermische Spaltung wurde aufgrund der Stereochemie der Sulphoxidgruppen und der mit den resultierenden Eliminationsprodukten verbundenen Belastung erörtert.

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Résumé Une étude thermogravimétrique d'une série de bis (sulfoxydes) de cyclophane (1–6) a montré que la décomposition thermique de ces composés se déroule en deux étapes avec pertes graduelles des groupes sulfoxydes à des températures de décomposition bien définies. Le clivage thermique graduel est expliqué par la stéréochimie des groupes sulfoxydes et la contrainte associée aux produits éliminés.

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Element-Element-Bindungen. I. Synthese und Struktur des Tetra(tert-butyl)tetrarsetans und des Tetra(tert-butyl)tetrastibetans

Element-Element Bonds. I. Syntheses and Structure of Tetra(tert-butyl)tetrarsetane and of Tetra(tert-butyl)tetrastibetane Dilithium (tert-butyl)arsenide reacts with (tert-butyl)dichloroarsine to give tetra-(tert-butyl)tetrarsetane 1 ; homologous tetra(tert-butyl)tetrastibetane 2 is formed by reduction of (tert-butyl)dichlorostibane with magnesium. The isotypic compounds 1/2 crystallize in the monoclinic space group P2₁/c with Z = 4. The dimensions of the unit cells determined at ?45 ± 5°C are: a = 957.4(8)/1 000.2(3); b = 1 399.1(14)/1 423.9(4); c = 1 697.4(9)/1 749.8(7) pm; β = 96.02(6)/96.77(3)°. As shown by low temperature X-ray structure determinations (3 531/3 232 symmetry independent reflections; R_g = 4.0/4.6%) the four membered rings E₄ (E = As or Sb) are folded; in all-trans configuration the bulky organic substituents occupy pseudo-equatorial positions. Characteristic averaged bond distances and angles are: E? E 244/282; E? C 202/221 pm; ? E? E? E 86/85° ? E? E? C 101/99°. The dihedral angels of the bisphenoides built up by the atoms of the rings are found to be 139/133°.     

Synthesis and Properties of Copper(II) Tetra(2-alkyl-4,5-benzimidazolo)- and Tetra(2,2'-Dimethyl-4,5-benzodiazepino)porphyrazines

4,5-Diaminophthalonitrile was reacted with carboxylic acids and acetylacetone to synthesize 2-alkyl-5,6-dicyanobenzimidazoles and 2,2'-dimethyl-5,6-dicyanobenzodiazepine, respectively. The products were converted into copper(II) porphyrazines. An effect of the heterocyclic residue on the physicochemical and spectral properties of the porphyrazines was revealed.     

5,10,15,20-四(对-癸酰氧基苯基)卟啉过渡金属配合物的合成与表征

液晶;5;10;15;20-四(对-癸酰氧基苯基)卟啉过渡金属配合物的合成与表征     

四（对—羟基苯基）卟啉过渡金属配合物的合成

四（对－羟基苯基）卟啉过渡金属配合物的合成师同顺＊柳巍刘国发王杏乔王世颖（吉林大学化学系长春１３００２３）关键词卟啉，过渡金属配合物，合成１９９７－１０－１７收稿，１９９８－０３－２０修回国家自然科学基金会资助四（对－羟基苯基）卟啉（Ｈ２ＴＨＰＰ）可...     

A Triply [5]Helicene-Bridged (1,3,5)Cyclophane

A rigid propeller-shaped conjugated triple macrocycle consisting of two nearly perfectly stacked benzene rings and three linking [5]helicene moieties has been synthesized using a glyoxylic Perkin approach. Analysis of the electron delocalization in this atypical aromatic molecule revealed global aromaticity and a 78 π-electron circuit along the edge of its triple loop, to the detriment of the two 6 π-electron circuits in the two stacked benzene rings.     

Synthesis and Complexation Studies of a Tetra(N,N-dimethyl) Aminoethylamide p-tert-butyl Calix[4]arene and Its Tetramethylammonium Derivative

We describe the synthesis of two functionalised p-tert-butyl calix[4]arenes: tetra(N,N-dimethyl) aminoethylamide derivative 1 and related tetramethylammonium 2. Their complexation properties towards alkali and zinc metal cations are reported along with complexation of perchlorate anion by 2.     

Multicyclic Polythioesters Derived from Pentaerythritol Tetra(mercaptoacetate)

Dry pentaerythritol tetra(mercaptoacetate), PETMA, was polycondensed with double molar amounts of phthaloyl chloride, isophthaloyl chloride, tetraphthaloyl chloride, adipoyl, suberoyl, sebacoyl and 1,10‐decanedioyl chloride. Pyridine served as HCl‐acceptor and catalyst. The concentration of PETMA was varied between 0.1 mol/L and 0.0125 mol/L. With the aromatic dicarboxylic acid, dichlorides gelation occurred in all experiments. With aliphatic dicarboxylic acid dichlorides (ADADs), soluble multicyclic polythioesters were obtained at concentrations of 0.025 or 0.0125 mol/L. These multicyclic polythioesters were characterized by viscosity measurements,¹H‐NMR spectroscopy and MALDI‐TOF mass spectrometry. A few experiments with pentaerythritol tetra(mercaptopropionate) showed a lower cyclization tendency relative to PETMA. Polycondensations of PETMA with α,ω‐dibromoalkanes or tri(ethylene glycol) bistosylate all ended with gelation.     

Synthesis and Crystal Structure of Tetra（o-cyanobenzyl）tin

The tetra（o-cyanobenzyl）tin compound has been synthesized by the reaction of cyanobenzyl chloride with tin, and its molecular structure was characterized by elemental analysis, IR spectra, ^1H NMR and X-ray diffraction. Crystal data for this compound： monoclinic, space group C2/c, Mr = 583.24, a = 1.9629（2）, b = 1.05967（13）, c = 1.41249（18） nm, β= 118.180（2）^o, V = 2.5898（5） nm^3, Z = 4, Dc =1.496 g/cm^3, μ（MoKa） = 1.015 cm^-1, F（000） = 1176, R = 0.0189, wR = 0.0497 （observed reflections with I 〉 20（I）） and R = 0.0218, wR = 0.0513 （all reflections）. The molecular structure adopts a distorted tetrahedral geometry around the tin atom. The Sn＇＂N weak interaction between the Sn and N atoms of cyano forms an intermolecular H-bonding, and the bond length is 0.3570 nm; the interaction between hydrogen of methylene and benzene ring of benzyl forms C-H…C with its bond length of 0.2817 nm; and the interaction among hydrogen of benzene ring and carbon of cyano forms Ph-H…C bond （0.2897 nm） Of the σ…π interaction. A 3D chain structure is formed by the above weak intermolecular interactions.     

Mit der Bestimmung von Tetra?thylblei (T?B) in dem Antiklopfmittel Tetra?thylbei-Fluid

Ohne Zusammenfassung