Synthesis and Crystal Structure of (3,6-Dichloro-2-nitrophenyl)(3-nitrophenyl)methanone

Novel compounds, (3,6-dichloro-2-nitrophenyl)(3-nitrophenyl)methanone(2), (2-amino-3,6-dichloro- phenyl)(3-aminophenyl)methanone(3) and 1-[3-(2-amino-3,6-dichlorobenzoyl)phenyl]-1H-pyrrole-2,5-dione(4), were synthesized from the initial compound 2,5-dichlorobenzophenone(1) and characterized by 1H NMR, 13C NMR, IR, mass spectrum and element analysis, respectively. The single crystal of compound 2 was obtained and determined by X-ray diffraction analysis. The single crystal data illustrates that it belongs to...     

2-[2-(6-Methylbenzothiazolyl)azo]-5-Diethylaminobenzoic acid as a new analytical reagent for the spectrophotometric determination of nickel

A new thiazolylazo chromogenic reagent, 2-[2-(6-methylbenzo-thiazoly)azo]-5-diethylaminobenzoic acid (6-Me-BTAEB), has been synthesized. Its chromogenic reaction with microamounts of nickel in the presence of sodium dodecylsulfate (SDS) has been thoroughly studied. 6-Me-BTAEB reacts with nickel(II) in weak acid medium containing appropriate amounts of SDS to form a blue-violet complex with high sensitivity, good selectivity and high stability. The composition is found to be 1:2 (nickel to 6-Me-BTAEB) and its absorption maximum is at 650 nm with an apparent molar absorptivity of 1.67 × 10⁵l mole^–1 cm^–1. Beer's law is obeyed over the range 0-0.4 g of nickel per ml. The proposed method has been applied to the direct determination of nickel in aluminium alloys, pure magnesium and low alloy steels at the 0.2–0.3% (w:w) level with satisfactory results.     

1-(4-硝基苯基)-3-(5-硝基-2-吡啶)-三氮烯的合成及其与汞(Ⅱ)的显色反应研究

合成了 1 -(4 -硝基苯基 ) -3 -(5-硝基 -2 -吡啶 ) -三氮烯 ,并研究了它与汞(Ⅱ )的显色反应。在TritonX -1 0 0的存在下 ,pH1 1 2的Na2 B4 O7-NaOH缓冲溶液中 ,试剂与汞生成 2∶1型桔黄色配合物 ,在 4 3 8nm和 52 5nm处分别有一正一负两个吸收波峰 ,用双峰双波长测定 ,其表观摩尔吸光系数为 2 1× 1 0 5L·mo1 1·cm 1,Hg2 +的浓度在 0～ 2 80 μg/L范围内符合比耳定律。成功地测定了人发和尿液中微量的汞。     

Synthesis and Crystal Structure of 1,2-Bis（2-benzimidazolyl）benzene

The title compound C6H4(C7H5N2)2 was prepared by the condensation of o-phenylenediamine with o-phthalic acid and characterized by elemental analysis, IR, UV and ^1H NMR spectra, and its structure was determined by single-crystal X-ray diffraction,showing the compound molecule belongs to (72 point group. A ID chain structure was formed by the intermolecular hydrogen bonds (N(2)H…N(I)).     

2-(2-喹啉偶氮)-5-二甲氨基苯酚光度法测定铀的研究

铀的测定一般采用铀试剂-Ⅲ或5-Br-PADAP光度法。2-喹啉偶氮类试剂已用于一些金属离子的测定,由于其共轭体系大,比吡啶偶氮类试剂具有更高的灵敏度。我们合成了2-(2-喹啉偶氮)-5-二甲氨基苯酚(QADMAP),产品经IR,MS及^1H NMR表征(谱图略)。研究其和铀的显色反应,建立了一种测定矿石中铀的方法。     

新试剂2-(5-硝基-2-吡啶偶氮)-5-二甲氨基苯甲酸分光光度法测定微量钴

本文报道用新试剂2-(5-硝基-2-吡啶偶氮)-5-二甲氨基苯甲酸分光光度法测定微量钴。配合物的表观摩尔吸光系数为1.31×10~5L·mol~(-1)·cm~(-1),Co∶5-NO_2-PAMB=1∶2,Co浓度在0～14μg/25mL范围内服从比耳定律。用于金属有机化合物中微量钴的测定,结果与理论值相符。     

Highly sensitive spectrophotometric determination of trace amounts of platinum(IV) with the molybdate-basic dyes-poly(vinyl alcohol) system

Three highly sensitive spectrophotometric methods for the determination of platinum(IV) have been developed, based on its colour reactions with molybdate and basic dyes (BD) in aqueous solution in the presence of poly(vinyl alcohol). Platinum(IV) reacts with molybdate and BD to form ion — association complexes of composition (BD)₂[Pt (MoO₄)₃]. The molar absorptivities are between 6.83 × 10⁵ and 9.51 × 10⁵ dm³mol^–1cm^–1, the highest value being found with nile blue. Suitable conditions for the reactions and the effects of foreign ions were investigated. The methods can be applied to the spectrophotometric determination of trace amounts of platinum(IV) in some catalysts and ores.     

微波辐射下双(2-苯并咪唑基)丙烷的合成与结构表征

与传统加热相比较,微波辐射促进的有机合成反应具有加热时间短、节能、产率高、不使用或少使用溶剂而对环境友好和节约成本等优点[1]。苯并咪唑类化合物具有广泛的生物活性而被应用到仿生有机合成、遗传学染色体研究及单层膜合成与形态研究的领域[2～4]。苯并咪唑类化合物的传统合成方法是:在HC1、多聚磷酸(PPA)、H3BO3等酸性催化剂使用下加热回流有机酸与邻苯二胺的混合物,然而反应通常需要较高的压力、温度或较长的时间,副反应多[5]。本研究在微波辐射下,以戊二酸和邻苯二胺为原料、PPA为催化剂合成了双(2-苯并咪唑基)丙烷,用正交试…     

1,5—二（2—氨基苯氧基）—N—苯基—3—氮杂戊烷的合成

合成了１，５－二（２－氨基（或硝基）苯氧基）－Ｎ－苯基－３－氮杂戊烷。对它们的结构作了元素分析、红外光谱、核磁共振谱及质谱鉴定。     

Synthesis, Crystal Structure and Nonisothermal Kinetics of Complex Co（tda）（5-mphen）（H2O）

The title complex,formulated as Co(tda)(5-mphen)(H2O)(H2tda=thiodiglycolic acid,5-mphen=5-methyl-1,10-phenanthroline),was synthesized and characterized by elemental analysis,IR spectroscopy,X-ray sin-gle crystal diffraction,and TG-DTG techniques. The complex crystallized in monoclinic space group C2/c,with parameters of a=1.8142(2) nm,b=0.78251(9) nm,c=2.4624(3) nm,β=93.809(2)°,V=3.4880(7) nm3,Z=8,Dc=1.579 g/cm3,the final R indices[I>2σ(I)] are R1=0.0469,wR2=0.1021,R indices for all data are R1=0.0835,wR2=0...     

Synthesis and electrical conductivity of poly(1,4-phenylenevinylene-co-2-nitro-1,4-phenylenevinylene)

A series of PPV copolymers containing 2-nitro-1,4-phenylenevinylene (NO₂-PV) units were prepared via the water-soluble precursor route. They were obtained in film form and were doped with I₂ and FeCl₃. Doping increased the electrical conductivities to maximum values of about 3×10^?2 and 3×10^?1 s cm^?1, respectively, for the two dopants. Conductivity depended strongly on the composition of the copolymers; it reached a maximum value at ca. 1–2 mol % of NO₂-PV units in the copolymers and then dropped rapidly with further increase in NO₂-PV content. Electronic effects of the substituent and morphological changes induced by copolymerization appear to interplay intricately, resulting in the occurrence of a maximum conducting composition. © 1993 John Wiley & Sons, Inc.     

Second derivative spectrophotometric method for simultaneous determination of cobalt, nickel and iron using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol

A simple, sensitive and rapid derivative spectrophotometric method using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) has been developed for simultaneous determination of Co(II), Ni(II) and Fe(II) which have very similar chemical behavior and appear together in many real samples. The complexes of all these metal ions with 5-Br-PADAP were formed immediately at pH 7.0 ammonium acetate buffered solution and were stable for at least 24 h. Second derivative spectra were selected for evaluation, because working wavelength determination was more precise and spectral overlap was less than in the ordinary and first derivative spectra. Three wavelengths at which the complexes exhibit extremum ²D values for Co(II), Ni(II) and Fe(II) were selected as analytical wavelengths, i.e., 640, 600 and 740 nm, respectively. Calibration curves drawn with zero-to-peak values at mentioned wavelengths were linear between 80 and 2000 ng ml⁻¹ for each metal ion. Concentrations of Co(II) and Ni(II) were calculated from the total ²D values and the sum of the linear equations for these three cations at 640 and 600 nm, after Fe(II) assay by making use of the ²D value at 740 nm. Limits of detection (LOD) for Co(II), Ni(II) and Fe(II) were 2.7, 13.9 and 3.0 ng ml⁻¹, respectively. The method has been applied to tool steel and heater resistance wire samples successfully.     

Synthesis and Crystal Structure of Binuclear Silver(Ⅰ)Complex with 2-nitro-(2-pyridylsulfanylmethyl)benzene

The reaction of 2-nitro-(2-pyridylsulfanylmethyl)benzene L with silver nitrate produces a centrosymmetric binuclear complex bis(2-nitro-(2-pyridylsulfanylmethyl)benzene-N,S)-bis(nitrato-O,O)-disilver(Ⅰ), [AgLNO3]2 1. The crystal is of triclinic, space group P1, with a = 7.383(3), b = 8.340(3), c = 12.003(4) A, a = 95.069(6), β = 93.498(5), γ = 102.734(6)°, C24H2oAg2N6-O10S2, Mr= 832.32, V= 715.6(4) A3, Z = 1, Dc = 1.931 g/cm3, F(000) = 412, μ = 1.581 mm-1, R=0.0351 and wR = 0.0749 Each silver atom is tetrahedrally coordinated by two O atoms from bidentate nitrate, one S atom from a ligand and one N atom from another ligand. Furthermore, AgAg interactions have been observed in the complex.     

5-(5-硝基-2-吡啶偶氮)-2,4-二氨基甲苯与铑显色反应的研究

本文报道以5-(5-硝基-2-吡啶偶氮)-2,4-二氨基甲苯(5-NO_2-PADAT)作分光光度法测定铑的新显色剂.结果表明,在PH 4.1及～6.5的乙酸-乙酸钠缓冲介质中,5-NO_2-PA-DAT与铑形成 2:1的紫红色络合物.该络合物在 1.8 mol/L高氯酸溶液中则转变为另一型体的蓝色络合物,最大吸收波长红移至583nm,表观摩尔吸光系数增至1.7×10_5L·mol_(-1)·cm(-1).以EDTA为掩蔽剂,大量的常见金属离子对测定无干扰.铑浓度在0～0.64μg/mL范围内遵守比尔定律.所建立的方法用于催化剂中微量铑的测定,结果满意.     

2－（5－Br－2－吡啶偶氮－5－二乙氨基）－酚与铑的显色反应的研究及应用

本文研究了２－（－５－Ｂｒ－２吡啶偶氮－５－二乙氨基）－酚与铑（Ⅲ）的显色反应。在ｐＨ为４．０的邻苯二甲酸氢钾缓冲液介质中，Ｒｈ（Ⅲ）与试剂形成稳定的橙红色络合物，其组成比为１：４，最大吸收波长为４９０ｎｍ，表现摩尔吸光系数为１．３×１０￣５Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）。铑含量在０～４μｇ／１０ｍＬ范围内服从比尔定律。     

酸性离子液体[Hnmp]HSO4催化下一锅三组分反应合成N-(2-羟基-1-萘基)(苯基)甲基-吡咯烷-2-酮衍生物

在无溶剂条件下,利用廉价无毒的酸性离子液体[Hnmp]HSO4为催化剂,醛、2-萘酚和吡咯烷酮一锅三组分合成了一系列新颖的N-(2-羟基-1-萘基)(苯基)甲基-吡咯烷-2-酮衍生物.与现有的方法相比该方法避免使用有机溶剂,且反应时间短,产率高,离子液体廉价易制备,且可回收重复再利用.     

Synthesis and Crystal Structure of Binuclear Silver(I) Complex with 2-nitro-(2-pyridylsulfanylmethyl)benzene

1 INTRODUCTION Metallosupramolecular species with metal-metal interactions have been designed and synthesized due to their potential applications as functional materi- als[1]. For Ag(I) coordination compounds, short Ag(I) –Ag(I) separations have been found in many bi- and polynuclear complexes[2~4], and these short metal- metal distances have been attributed to the ligand ar- chitecture[5, 6]. Thus, the rational design of bi- and polynuclear Ag(I) complexes must recognize the in- here…     

Synthesis and characterization of 2-(5-Bromo-2-Pyridylazo)-5-[(N,N-dicarboxylmethyl) amino]- phenol as a water-soluble chromogenic reagent

A new water soluble chromogenic reagent, 2-(5-bromo-pyridylazo)-5-[(N,N-dicarboxylmethyl)amino]-phenol has been synthesized. Its colour reaction with various metal ions was tested, and the acid dissociation constant of the reagent, and the stability constants of the chelates of Ni²⁺, Co²⁺, Cu²⁺, Mn²⁺, Pb²⁺, Zn²⁺ and UO ₂ ²⁺ were determined. The application of the reagent to spectrophotometric determination of nickel in irons is presented.     

新型苯基噻吩-2-基甲酮类化合物的合成及其对人脐静脉内皮细胞的保护活性

合成了13个具有新型结构的苯基(噻吩-2-基)甲酮类化合物,其中3个化合物(9b,10b,11b)未见文献报道,目标化合物的结构均经ESI-MS、1H NMR和13C NMR等技术手段进行了确证。 对H2O2诱导的人脐静脉内皮细胞(HUVECs)氧化损伤保护活性的结果显示,对位甲氧基以及两个氯原子取代的活性较好。 初步构效关系表明,苯基噻吩甲酮母环上取代基的位置、数目、类型是影响化合物活性的主要原因。     

Synthesis and bioactivity of novel (3-chloro-5-(trifluoromethyl)pyridin-2-yloxy)phenyl containing acrylate and acrylonitrile derivatives

Fifteen novel (3-chloro-5-(trifluoromethyl)pyridin-2-yloxy)phenyl containing Baylis-Hillman adduct derivatives were designed and synthesized. Evaluation of their biological activities showed that methyl 2-((3-(3-chloro-5-(trifluoromethyl)pyridin-2-yloxy)phenoxy)(phenyl)methyl)acrylate (2g) exhibited efficient broad-spectrum fungicidal activity, with 100% control of wheat powdery mildew and cucumber downy mildew and 98% control of cucumber anthracnose at 400 g ai/ha. Some of the other title compounds 2, 3 and two Baylis-Hillman bromide intermediates (11a, 11b) had moderate to good fungicidal activity.