Polyethylene glycol (PEG-400) promoted one-pot,five-component synthesis of (E)-ethyl2-(2-((E)-2-(1-(4-methyl-2-(phenylamino)thiazol-5yl)ethylidene)hydrazinyl)-4-oxothiazol-5(4H)-ylidene)acetates

Molecular Diversity - A facile, inexpensive and eco-friendly synthesis of functionalised...     

5-(4-氯苯基偶氮)-8-苯磺酰氨基喹啉分光光度法测定微量镍(Ⅱ)

在 p H10 .5的 Na2 B4O7- Na OH介质及 CS(NH2 ) 2 、氯化十六烷基吡啶 (CPC)存在时 ,室温下镍 ( )与5 - (4 -氯苯基偶氮 ) - 8-苯磺酰氨基喹啉 (CPBSQ)反应 ,生成络合比为 1∶ 4的有色络合物 ,其最大吸收波长位于 6 0 0 nm。研究了反应的最佳条件 ,建立了一个测定 Ni( )的光度分析新方法。 Ni( )的浓度在 0—10 .0 μg/2 5 m L范围内符合比耳定律 ,其摩尔吸光系数为 1.93× 10 5L· mol-1·cm-1。考察了 2 0多种共存离子的影响 ,大多数常见离子在氨水沉淀分离后不干扰测定。方法用于合金钢中镍的测定 ,其相对标准偏差为 1.9%— 2 .1% ,标准加入回收率为 97%— 10 4 %。     

Structural analogy between GeSi(111)-5 × 5 and Si(111)-7 × 7 surfaces

Low energy electron diffraction (LEED) patterns for the GeSi(111)-5 × 5 surface are reported and compared to those for the Si(111)-7 × 7 surface. Parallels between the observed LEED patterns are explained by a structural analogy between GeSi(111)-5 × 5 and Si(111)-7 × 7 surfaces. Both the (5 × 5) and (7 × 7) patterns are shown to be consistent with structural models of the triangle-dimer type previously proposed for Si(111)-7 × 7 surface.     

吡啶衍生物研究(Ⅰ)3-(4-吡啶基)-4-烷(芳)基-1,2,4-三唑啉-5-硫酮的NMR研究

研究并归属了十七个3-(4-吡啶基)-4-烷(芳)基-1,2,4-三唑啉-5-硫酮的¹HNMR和¹³C NMR化学位移,讨论了影响化学位移的主要因素.     

5-(偶氮苯)-8-(4-硝基-1-重氮苯)-氨基喹啉与铜显色反应研究应用

研究了新试剂5－（偶氮苯）－8－（4－硝基－1－重氮苯）－氨基喹啉（PANPAQ）与铜的显色反应，在弱碱性介质中，吐温－80存在下，PANPAQ与Cu（Ⅱ）反应生成2：1紫色络合物，λmax＝615nm，ε＝5.19×10^4L·mol^-1·cm^-1，铜含量在0－15μg/25mL内符合比耳定律，方法用于生物样品中铜的测定，结果满意。     

2-(2-喹啉偶氮)-5-二甲氨基苯胺光度法测定铜

在pH=4.0的磷酸盐缓冲介质中,CTMAB存在下,2-(2-喹啉偶氮)-5-二甲氨基苯胺(QADMAA)与铜反应生成2:1稳定络合物,络合物λmax=580nm,ε=1.14×105L·mol-1·cm-1.铜含量在0.01-0.6μg/mL内符合比耳定律,方法用于环境样品中铜的测定,结果令人满意.     

Experimental and theoretical determination of transition dipole moments of ethyl 5-(4-aminophenyl)- and 5-(4-dimethylaminophenyl)-3-amino-2,4-dicyanobenzoate

The absorption and fluorescence transition dipole moments ( $\hat M_{ge}$ and $\hat M_{eg}$ ) for ethyl 5-(4-aminophenyl)-3-amino-2, 4-dicyanobenzoate (EAADCy) and ethyl 5-(4-dimethylaminophenyl)-3-amino-2, 4-dicyanobenzoate (EDMAADCy) have been determined on the basis of the steady-state and time-resolved spectroscopic measurements and semiempirical quantum-chemical calculations. The values of the transition dipole moments of perpendicular and flattened forms of the investigated molecules were estimated as a function of the solvent polarity. Noted differences between the absorption and emission transition dipole moments (i.e., ${{\hat M_{ge} } \mathord{\left/ {\vphantom {{\hat M_{ge} } {\hat M_{eg} }}} \right. \kern-0em} {\hat M_{eg} }} \ne 1$ ) confirm that the change of the electronic and molecular structure take place in the excited state.     

新型锌离子荧光探针(5-(二甲基氨基)-N-(4-(2-(2-喹啉亚甲基)甲酰肼基)苯基)萘-1-磺酰胺)的研究

以丹磺酰胺为荧光基团设计合成了新型Zn²⁺荧光探针DW1(5-(二甲基氨基)-N-(4-(2-(2-喹啉亚甲基)甲酰肼基)苯基)萘-1-磺酰胺)。通过紫外光谱、荧光光谱及电喷雾质谱研究了DW1对Zn²⁺的选择性识别作用。结果表明,DW1与Zn²⁺结合后荧光显著增强,荧光发射光谱由545 nm蓝移至515 nm,量子产率达到0.32,且对Zn²⁺具有较高的选择性,受常见离子的干扰较小。光谱滴定和ESI-MS谱表明DW1与Zn²⁺以1∶1的化学计量数形成配合物,平衡常数K=1.75×10⁴(mol/L)^-1。     

Spectroscopic Studies of Intramolecular Proton Transfer in 2-(4-Fluorophenylamino)-5-(2,4-Dihydroxybenzeno)-1,3,4-Thiadiazole

Spectroscopic studies of the biologically active compound 2-(4-fluorophenylamino)-5-(2,4-dihydroxybenzeno)-1,3,4-thiadiazole (FABT), have been performed. Absorption studies in the UV-Vis region for FABT in polar solvents, like water or ethanol, exhibit the domination of the enol form over its keto counterpart, with a broad absorption band centered around 340 nm. In non-polar solvents such as n-heptane or heavier alkanes the 340 nm absorption band disappears and an increase of the band related to the keto form (approximately 270 nm) is observed. Fluorescence spectra (with 270 nm and 340 nm excitation energies used) show a similar dependence: for FABT in 2-propanol a peak at about 400 nm dominates over that at 330 nm while in n-heptane this relation is reversed. The solvent dependent equilibrium between the keto and enol forms is further confirmed by FTIR and Raman spectroscopies. As can be expected, this equilibrium also shows some temperature dependences. We note that the changes between the two tautomeric forms of FABT are not related to the permanent dipole moment of the solvent but rather to its dipole polarizability.     

Synthesis of( E ) -5- ( dimethylamino ) -N- ( 4- ( 2- ( quinolin-2-ylmethylene ) -hydrazinecarbonyi ) phenyl ) naphthalene-1-sulfonamide for Detection of Zinc Ion

以丹磺酰胺为荧光基团设计合成了新型Zn2+荧光探针DW1(5-(二甲基氨基)-N-(4-(2-(2-喹啉亚甲基)甲酰肼基)苯基)萘-1-磺酰胺).通过紫外光谱、荧光光谱及电喷雾质谱研究了DW1对Zn2+的选择性识别作用.结果表明,DW1与Zn2+结合后荧光显著增强,荧光发射光谱由545nm蓝移至515nm,量子产率达到0.32,且对Zn2具有较高的选择性,受常见离子的干扰较小.光谱滴定和ESI-MS谱表明DW1与Zn2+以1:1的化学计量数形成配合物,平衡常数K=1.75×104(mol/L)-1.     

Surface structure of SrTiO3(100)-(square root of 5 x square root of 5) - R26.6 degrees

Atomic and electronic structures of the SrTiO3(100)-(square root of 5 x square root of 5) - R26.6 degrees surface are studied by using scanning tunneling microscopy (STM) and noncontact atomic force microscopy (NC-AFM). Instead of the well established oxygen vacancy model, it is found that a structural model, consisting of an ordered Sr adatom at the oxygen fourfold site of a TiO2 terminated layer, can explain the experimental results very well. We theoretically simulate the model cluster with the first-principles total-energy calculation. Calculated density of states and images for STM and NC-AFM are in good agreement with the experimental results.     

应用NMR技术确证5-(R)-(1-孟氧基)-2(5H)-呋喃酮与苯甲醛肟1,3-偶极环加成产物的结构

5-(R)-(l-孟氧基)-2(5H)-呋喃酮(A)与苯甲醛肟(B)进行1,3-偶极环加成反应时得到两个产物, 我们应用NOE及HMBC技术确证了它们的结构. 由于反应物(A)的绝对构型已经X-射线单晶衍射法确证, 因此通过NMR研究产物呋喃酮环上各手性碳的关系, 最终确立产物的绝对构型.     

2,4—二氨基—6—(取代苄基)—5—甲基吡啶(2,3d)并嘧啶类化合物的~(13)C NMR研究

2,4-二氨基-6-(取代苄基)-5-甲基吡啶(2,3d)并嘧啶类化合物是一类很有前途的抗癌新药。本文研究了24种7位氯代和氧代的该类化合物的碳谱,归属了母核及取代苄基上各碳的化学位移,并对两种取代对母核碳上的化学位移的影响规律进行了探讨,文中所有数据迄今未见文献报道。     

Intramolecular energy and charge transfer in 5-(9-anthryl)-3-(4-nitrophenyl)-1-phenyl-2-pyrazoline

The absorption and photoluminescence of the newly synthesized 5-(9-anthryl)-3-(4-nitrophenyl)-1-phenyl-2-pyrazoline (AN PP) were investigated. The absorption is the absorption of anthryl moiety at about 325-400 nm, superimposed on the broader absorption of 3-(4-nitrophenyl)-1-phenyl-2-pyrazoline moiety peaked at 420 nm. On excitation at 420 nm, the fluorescence spectrum has only one emission band from the pyrazoline moiety. This emission band exhibits a larger red shift with an increase in the polarity of solvents. But on excitation at 365 nm, the fluorescence spectrum has two emission bands coming from the anthryl and pyrazoline moieties, respectively. The intensity ratio of the two bands is different in solvents of different polarity. It is concluded that photo-induced intramolecular energy transfer from the anthryl to pyrazoline moiety exists simultaneously with the charge transfer from N (1) to C (3) in the pyrazoline moiety in the excited state and both compete with each other.     

(2R,5S)-N-间氟苄基-2,5-二甲基哌嗪的合成

以(2R,5S)-2,5-二甲基哌嗪为原料,经过成盐,单取代反应,用D-酉石酸对光学异构体的手性拆分,用氢氧化钠游离,最终合成(2R,5S)-N-间氟苄基-2,5-二甲基哌嗪,反应总收率为83％.该物质的合成未见文献报道,目标化合物用1H NMR,IR进行结构表征.     

应用NMR技术确证5-(R)-(l-氧基)-2(5H)-呋喃酮与苯甲醛肟1,3-偶极环加成产物的结构

5 (R) (l 艹孟 氧基 ) 2 (5H) 呋喃酮 (A)与苯甲醛肟 (B)进行 1 ,3 偶极环加成反应时得到两个产物 ,我们应用NOE及HMBC技术确证了它们的结构 .由于反应物 (A)的绝对构型已经X 射线单晶衍射法确证 ,因此通过NMR研究产物呋喃酮环上各手性碳的关系 ,最终确立产物的绝对构型 .     

新试剂2-(4安替比林偶氮)-5-二甲氨基苯胺与铜显色反应的研究

在pH=4.5HAc-NaAc缓冲介质中，吐温－80存在下，2－（4安替比林偶氮）－5－二甲氨基苯胺（ADA）与铜生成2：1红色络合物，λmax=520nm,ε=5.24×10^4L·mol^-1·cm^-1。铜含量在0－20μg/25mL内符合比耳定律，方法用于食品中铜的测定，结果满意。     

5-(2-苯并噻唑偶氮)-8-氨基喹啉作为钴的光度分析试剂及应用研究

在阳离子表面活性剂溴化十六烷基三甲基铵存在下 ,于 p H=9.2的硼砂缓冲介质中 ,5 - (2 -苯并噻唑偶氮 ) - 8-氨基喹啉与钴 ( )形成 2∶ 1的蓝色配合物 ,其最大吸收波长位于 6 5 0 nm处 ,表观摩尔吸光系数为 1.2 4× 10 5L· mol-1· cm-1。钴浓度在 0— 10 .0μg/2 5 m L范围内 ,符合比耳定律。应用于维生素 B12 和水系沉积物中微量钴的测定 ,获得了满意的结果。