Highly Sensitive Spectrofluorimetric Determination of Trace Amounts of Indium(Ⅲ) with Salicylaldehyde Salicyloylhydrazone

The fluorescent reaction of salicylaldehyde salicyloylhydrazone(SASH) with indium(Ⅲ) was studied in detail. Based on this chelation reaction, a sensitive spectrofluorimetric method was developed for the determination of indium in a water ethanol(volume ratio 3∶7) medium at pH 4 0. Under the condition, the In SASH complex displays an excitation and emission maxima at 396 and 461 nm, respectively. The linear range of the method is from 4 7 to 1000 ng/mL and the detection limit is 0 94 ng/mL. The molar ratio of indium to the reagent is 1∶1. The interferences of other ions were studied. The method was successfully applied to the determination of indium in the chemical reagents of lead, tin, zinc, zinc chloride and geological samples by standard addition method.

Spectrofluorimetric Determination of Trace Amounts of Gallium with Salicylaldehyde Benzoylhydrazone

The fluorescent reagent salicylaldehyde benzoylhydrazone(SABH) was synthesized and its ionization constants were estimated spectrophotometrically. The fluorescent reaction of this reagent with gallium was studied. Based on this chelation reaction, a spectrofluorimetric method was developed for the determination of gallium in a water medium at pH 3.2. Under these conditions, the Ga SABH complex has excitation and emission maxima at 372 and 455 nm, respectively. The linear range of the method was 0～150 μg/L and the detection limit was 0.36 μg/L of gallium when a standard addition method was used in the assay. The molar ratio of gallium to the reagent was 1∶3. The interference of other ions was studied. The extraction with n butyl acetate from a 6 mol/L hydrochloric acid medium was used to separate Ga from the interfering elements in semiconductor silicon and geological samples, and themethod has been successfully applied to the determination of gallium in these samples.

Synthesis, Characterization and Thermodecomposition Kinetics of Terbium(Ⅲ) Complex with Novel Schiff Base Salicylaldehyde-Taurine and 1,10-Phenanthroline

A complex of terbium(Ⅲ) with Schiff base salicylaldehyde-taurine and 1,10-phenanthroline was synthesized. The molecular formula was [Tb (sal-taurine) (1,10-phen) (NO_3)]·2H_2O (sal=salicylaldehyde, 1,10-phen=1,10-phenanthroline). The composition of the title complex was determined by elemental analysis and EDTA volumetic analysis. IR, Molar conductivity and X-ray powder diffraction were performed for its characterizations. The thermal decomposition kinetics of the complex were investigated under non-isothermal condition using the Achar differential method and the Coats-Redfern integral method. The kinetic equation for the second step corresponds to the mechanisms of the Zhuralev, Lesokin and Templman equation were obtained.

Microcalorimetric Character of Inhibition of Salicylaldehyde Glucosamine Schiff Base SG on Bacterial Metabolism

The power time curves of the reaction of E.coli with SG at different temperatures were determined by microcalorimetric method and the mutliplication rate constant k , generation time G , ratio I , and thermogenetic quantity Q , Q 0 and 0 were calculated.The function formulas have been established. It was found that P max , t g, t and 0 can be used to characterize the bacterial growth metabolism of E.coli and the antibacterial activity of SG.

Microwave Preparation and Spectroscopic Investigation of Binuclear Schiff Base Metal Complexes Derived from 2,6-Diaminopyridine with Salicylaldehyde

The binuclear Schiff base complexes prepared by condensation 2,6-diamino-pyridine and salicylaldehyde (LH) by using microwave and adding metal salts to ligand by same ratio. The Schiff base ligand was checked by infrared, electronic spectra and 1HNMR spectroscopy and prepared complexes characterized by molar conductivity, infrared, electronic spectra and susceptibility measurements. The values of molar conductivities reveal that the complexes are non-electrolytes, from obtained data of electronic spectra and magnetic moment, an octahedral geometry was suggested, coordinated to the metal ions in a manner with N donor sites of imine groups, and oxygen of phenolic OH group.

Ultrasonic-assisted condensation of chitosan with salicylaldehyde

In order to synthesize an improved adsorbent for heavy metal ions,we studied the condensation reaction of chitosan with salicylaldehyde in ethanol to form a Schiff base.The effect irradiating the reaction using an ultrasonic liquid processor was contrasted with conventional methods.The IR spectra of condensed chitosan prepared by the two methods showed that their molecular structures were identical.The reaction conditions,including solvents,ultrasonic power density and irradiation time,pH,and reactant ratio,were optimized by orthogonal design.A shorter reaction time and a higher product yield were obtained using ultrasonic-assisted synthesis compared with the traditional method.A condensation degree of 89.63% was achieved using the optimized conditions:i.e.ultrasonic irradiation at 180 W for 60 min;95% ethanol as the solvent,pH 4.0,and salicylaldehyde:chitosan ratio of 6:1.

Crystal Structures of O－Vanillin－semicarbazide and Salicylaldehyde－semicarbazide

o-Vanillin-semicarbazide C_9H_(11) N_3O_3, written simply as cpl, M_r= 209. 21 is a yellow crystal. Cp1 crystallizes in the monoclinic space group P2_1/a with unit cell parameters: a= 6. 596(6) , b=20. 534(6) , c=7. 108(6) , β=99.00(8)°,Z=4, D_c=1. 46 g/cm￣3, V=951 , μ=1. 05cm￣(-1), F(000)=440, R=0. 058, R_w =0. 056. Salicylaldehyde-semicarbazide C_8H_9N_3O_2, written simply as cp2, M_r=179.18 is a colorless crystal. cp2 crystallizes in the triclinic space group P1 with a= 5.276 (3), b=7. 116(4) , c=24. 286(3), a=86. 72(3) ,β=83. 99(3),γ=68.22(5) °,Z=4 , D_c=1. 41 g/cm￣3, V=841.9,μ=0. 98 cm ￣(-1),F (000)=376, R=0.066,R_w= 0. 067. The dihedral angle between plane 1 formed by benzene ring and plane 2 by N(2) , C(2), N(3), and O(3) is 161.40°for cp1, while the angle between plane 3 made by benzene ring (or benzene ring in the other molecule)and plane 4 by N(2) , C (18) , N(3) and O(3) For N(5),C(28) , O(4) , and N(6)]is 15. 07°(or 15. 15°) for cp2. The temperature of the thermodecomposition of cp1 is higher than that of cp2.

Optical Properties, Electronic Energy Level Structure and Electroluminescent Characteristics of Salicylaldehyde Anil Zinc

A new electroluminescent material, salicylaldehyde anil zinc （SAZ） was synthesized, which can form high quality, thermal stability, nano-scale amorphous films by vacuum evaporation. Its structure, thermal stability were characterized by infrared （IR） spectra, differential thermal analysis-thermogravimetry （DTA-TG） analysis, respectively. The optical properties of SAZ were investigated by UV absorption spectra, Photoluminescence （PL） excitation and emission spectra. The highest occupied molecular orbits （HOMO）, lowest unoccupied molecular orbits （LUMO） and optical band gap were evaluated by cyclic voltammetry curve and optical absorption band edge. The electroluminescent devices using SAZ as the emissive layer emit green light with a peak wavelength at 509 nm and a brightness of about 3.1 cd/m^2.

Synthesis, Characterization, Thermal Decomposition Mechanism and Non-Isothermal Kinetics of Salicylaldehyde Salicylhydrazone and Its Complex of Erbium(Ⅲ)

The salicylaldehyde salicylhydrazone and its complex of Er(Ⅲ) were synthesized. The formulae K·4H_2O(HL=[C_(14)H_(10)N_2O_3]^(2-), the bivalent form of the salicylaldehyde salicylhydrazone) were determined by elemental analysis and EDTA volumetric analysis. Molar conductance, IR, UV and X-ray power diffraction were carried out for the characterizations of the complex and the ligand. There are two stable five-numbered and six-numbered circles in the complex. The thermal decompositions of the ligand and the complex with the kinetic study are carried out by non-isothermal thermogravimetry. The stages of the decompositions were identified by TG-DTG curve. The non-isothermal kinetic data were analyzed by means of integral and differential methods. The possible reaction mechanism and the kinetic equation were investigated by the corresponding kinetic parameters.The activation energy value of the main step decomposition are also calculated by Kissinger′s method and Ozawa′s method.

Synthesis and spectral studies of macrocyclic Pb(Ⅱ),Zn(Ⅱ),Cd(Ⅱ)and La(Ⅲ) complexes derived from 1,4-bis(3-aminopropoxy)butane with metal nitrate and salicylaldehyde derivatives

Eight new macrocyclic complexes were synthesized by template reaction of 1,4-bis（3-aminopropoxy）butane with metal nitrate and 1,3-bis（2-formylphenyl）propane or 1,4-bis（2-formylphenyl）butane and their structures were proposed on the basis of elemental analysis, FTIR, UV-vis, molar conductivity measurements, ^1H NMR and mass spectra. The metals to ligand molar ratios of the complexes were found to be 1： 1. The complexes are 1：2 electrolytes for Pb（II）, Zn（II） and Cd（II） complexes and 1：3 electrolytes for La（III） as shown by their molar conductivities （Am） in DMSO at 10^-3 mol L^-1. Due to the existence of free ions in these complexes, such complexes are electrically conductive. The configurations of La（III） and Pb（II） were proposed to probably octahedral and Zn（II） and Cd（II） complexes were proposed to probably tetrahedral.

A Novel Potassium Complex Based on the Taurine-salicylaldehyde Schiff Base:Synthesis,Crystal Structure and Spectroscopy

A novel two-dimensional self-assembly network formulated as [K（TSSB）]n （TSSB= taurine-salicylaldehyde Schiff base） has been synthesized via the reaction of salicylaldehyde with taurine at the presence of potassium hydroxide in water-methanol solution,and was structurally characterized by elemental analysis,IR,UV-VIS spectra and X-ray diffraction.It crystallizes in the monoclinic system,space group P21/c with a=20.245（3）,b=7.2905（9）,c=7.5458（10）,β= 94.1920（10）o,V=1110.8（2）3,Mr=267.34,Z=4,Dc=1.599 g/cm3,μ（MoKα）=0.663 mm-1 and F（000）=552.The units of K[TSSB] are linked into a one-dimensional double chain structure via the sulfonic groups from the taurine-salicylaldelyde Schiff base,and such chains are further extended through O-K-O bond interactions resulting in a two-dimensional supramolecular architecture.In the complex,the K（I） ion displays a slightly distorted dodecahedral geometry with an eight-coordination number.

Highly Sensitive Spectrofluorometric Determination of Trace Amount of Gallium with Salicylaldehyde-5-bromo-salicyloylhydrazone

オhe fluorescent reagent, salicylaldehyde-5-bromo-salicyloylhydrazone (SABSH) was synthesized and its ionization constants were determined spectrophotometrically. The fluorescent reaction of this reagent with gallium was studied. Based on this chelation reaction, a highly sensitive spectrofluorometric method was developed for the determination of gallium in a ethanol-water (3+2, V/V) medium at pH 2.3. Under these conditions, the GaⅢSABSH complex has excitation and emission maxima at 390 and 457 nm, respectively. The linear range of the method is from 0.0 to 1×10-4 g/L and the detection limit is 4×10-7 g/L of gallium when a standard additions method is used. The molar ratio of gallium to the reagent is 1∶1. Interferences were evaluated. The method was successfully applied to the determination of gallium in soil samples. Extraction with n-butyl acetate from 6 mol/L hydrochloric acid medium was used to separate gallium from the interfering elements in the soil samples.

Polymerization of Butyl Methacrylate Catalyzed by Salicylaldehyde-Imine Zirconium/Al(i-Bu)_3 System

A new kind of zirconium（Zr） complex containing ligand of salicylaldehyde-imine was successfully synthesized with ZrCl_4·2 THF and salicylaldehyde-imine as raw materials. The ligand was characterized by means of ~1HNMR, IR, and GC-MS, and Zr complex was characterized by means of ~1HNMR and IR, respectively. The Zr complex, combined with co-catalyst of Al（i-Bu）_3, was explored to be effective catalytic system for the polymerization of butyl methacrylate（BMA）, to prepare poly-n-butyl methacrylate（PBMA）, which was characterized by IR, ~13C-NMR and GPC. Compared with other double-component（MAO/Cat, AlEt_3/Cat） catalytic systems, catalytic system of Al（i-Bu）_3 and the Zr complex provided the best catalytic activity under the same conditions. The influence of polymerization parameters, such as molar ratio of Al（i-Bu）_3/Cat and BMA/Cat, polymerization temperature and polymerization time, was studied with Zr complex/Al（i-Bu）_3 system. With increasing polymerization time from 4 to 24 hour, the monomer conversion increased from 40.14% to 96.56%. Viscosity-average molecular weight（M_v） of PBMA, detected by the viscosity methodology, increased from 12.67×10~4Da to 44.97×10~4Da and lower molecular weight distribution was obtained. According to these results, the Zr complex contained ligand of salicylaldehyde-imine was a kind of readily, long lifetime and high activity catalyst for BMA polymerization.

氯球嫁接L-脯氨酸绿色催化合成香豆素-3-羧酸酯

将L-脯氨酸嫁接在树脂氯球上,催化水杨醛及其衍生物和丙二酸酯直接合成香豆素-3-羧酸酯类物质,反应具有选择性强、产率高、成本低、三废少、后处理简单、催化剂可以多次重复使用等优点,符合绿色催化的特性。实验表明:反应在100℃下,醛和酯的摩尔比为1:1.2,催化剂的用量1 g,10 mL DMF中反应5h,反应的选择性≥98%,产率高达92%;催化剂循环使用6次反应的产率仍在85%以上。在此优化的反应条件下,高效合成了一系列其他香豆素-3-羧酸酯类物质,产品的结构和纯度通过了NMR、IR和熔点等手段进行了鉴定。

24种植物精油对德国小蠊的驱避活性

为评估不同植物精油对德国小蠊的驱避活性,进而筛选出驱避效果最佳的植物源驱避剂,为开发新型蟑螂驱避类产品提供参考。采用三连筒测试法进行试验,间隔相同时间对三连筒内德国小蠊的分布状况进行观察并选出效果更佳的植物精油,再用Y型嗅觉仪进一步确定其驱避活性。试验结果表明,在1.2500μL·cm^(-2)剂量下,每2 min对三连筒内德国小蠊的分布状况进行记录,发现24种植物源驱避剂中,水杨醛和桂醛2种植物源驱避剂的驱避效果较显著。对2种植物源驱避剂设置剂量梯度进一步试验,结果表明,驱避率随着浓度的降低而降低。在0.6250μL·cm^(-2)剂量下,2种植物源驱避剂在空气中流动后,三连筒内德国小蠊的分布状况都发生明显变动,均有大部分德国小蠊向远离植物源驱避剂悬挂端移动。在0.3125μL·cm^(-2)剂量下,水杨醛和桂醛对德国小蠊的驱避率均在50%以上,效果仍不错。三连筒试验结束后,再用Y型嗅觉仪对相同浓度的植物精油进行试验,发现水杨醛和桂醛对德国小蠊的驱避率与三连筒试验中的结果相近。综上,水杨醛和桂醛对德国小蠊有较好的驱避效果,具有作为蟑螂驱避类产品的应用前景。

水杨醛席夫碱Pd配合物的合成、表征及催化Suzuki偶联反应研究

以水杨醛和2-氯-4-氟苯胺合成的席夫碱为配体,采用溶剂热法生成新型Pd(Ⅱ)配合物(Ⅰ)。利用傅里叶红外、热重、PXRD、X-射线单晶衍射等测试手段对其进行结构表征与性质研究。结果表明,配合物(Ⅰ)在P2_(1)/c空间群中属于单斜晶系,通过亚胺N和酚O供体原子以双齿方式与1个钯(Ⅱ)中心配合。以制备的Pd(Ⅱ)配合物为催化剂,考察其催化溴苯与苯硼酸Suzuki偶联反应的反应条件,当催化剂摩尔分数为2%、K_(2)CO_(3)为助催化剂、EtOH为溶剂、反应温度为80℃、反应时间为6 h时催化产率高达99.6%。考察不同反应底物的催化反应效果,结果表明,含吸电子基团的卤代芳烃表现出更好的催化性能,且溴苯与苯硼酸反应的催化效果最佳。

1-(3-氟苯基)-2-(6-甲氧基-2-(1-(3,4,5-三甲氧基苯基)乙烯基)苯并呋喃-5-基)乙烯合成工艺优化及活性初探

以4-甲氧基水杨醛为原料、乙腈为溶剂,通过溴代、碘代、Rap-Stoermer偶联、Heck偶联4步反应合成了目标化合物1-(3-氟苯基)-2-(6-甲氧基-2-(1-(3,4,5-三甲氧基苯基)乙烯基)苯并呋喃-5-基)乙烯,通过单因素实验对关键步骤碘代反应条件进行了优化,通过^(1)HNMR、^(13)CNMR、MS对目标化合物的结构进行了表征,并对目标化合物的微管蛋白和PI3K双靶点抑制活性进行了初步研究。结果表明,碘代反应最佳条件为:以对甲苯磺酸一水合物为催化剂、反应温度25℃、反应时间10 h、碘代试剂用量n(4-甲氧基水杨醛)∶n(N-碘代丁二酰亚胺)为1∶1.0、溶剂用量n(4-甲氧基水杨醛)∶V(乙腈)为1∶3(mmol∶mL),在此条件下碘代反应产率为70.6%;通过分子对接验证了目标化合物具有双靶点抑制活性,其对微管蛋白的抑制活性高于对PI3K的抑制活性。

对羟基苯甲醛Schiff碱的合成、表征及生物活性

Schiff是优良配体,并具有抑菌、抗氧化和抗肿瘤等生物活性。以对羟基苯甲醛为原料,分别与4-甲基、5-甲基-2-氨基吡啶反应,合成了2个对羟基苯甲醛Schiff碱,即对羟基苯甲醛缩4-甲基-2-氨基吡啶(1)和对羟基苯甲醛缩5-甲基-2-氨基吡啶(2)。采用熔点、红外光谱、紫外可见光谱、核磁共振氢谱和碳谱以及高分辨质谱等对产物结构进行了全面表征。利用微量肉汤稀释法研究其抑菌活性,结果标明:化合物1和化合物2对大肠杆菌、金黄色葡萄球菌和枯草芽孢杆菌的最小抑菌浓度(MIC)为0.500 mg/mL,对溶藻性弧菌、副溶血性弧菌的MIC为0.250 mg/mL。采用DPPH·法研究了化合物1的抗氧化活性,发现其对DPPH·自由基清除率为68.1%。

Synthesis and Crystal Structure of Tri(4-(3-hydroxy2-ethyl-4-pyridinone-1-yl)-aniline Condensation Salicylaldehydato) Monohydratotricopper(II)Dimethylformamide Monohydrate Solvate

The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H15N2O3)3(H2O)]DMFH2O. The coordi- nation sphere about each copper ion in the complex consists of two oxygen atoms from hydroxylpyridinone moiety of one ligand and one oxygen and one nitrogen atoms from salicyladehyde Schiff-base moiety of another ligand arranged in a slightly distorted square planar geometry. Among the three copper ions, one (Cu(2)) is coordinated by the other oxygen atom of water molecule on the fifth coordinate position to form a distorted square pyramid geometry. The crystal is of monoclinic, space group P21/c with a = 12.9202(5), b = 27.197(1), c = 17.0116(7) ? b = 100.588(1), V = 5875.9(4) 3, Z = 4, C63H57N7O12Cu3, Mr = 1294.78, Dc = 1.464 g/cm3, m = 1.146 mm-1, F(000) = 2668, R = 0.0784 and wR = 0.1546 for 6926 observed reflections with I > 2s(I). The differences of coordinate bond lengths are observed between anhydrous and hydrous units: in the former unit, the average bond lengths are 1.978 ?for CuN (azomethine), 1.883 ?for CuO (phenolic) in Schiff-base moiety, 1.959 ?for CuO (keto), and 1.919 ?for CuO (hydroxy) in hydroxypyridinone moiety; while those in the latter are longer with the following corresponding values: 1.985(5), 1.908(5), 1.993(5) and 1.919(4) ? respectively. The Cu(2)O (water) bond length is 2.375(6) ?