[Ni(py)3(SHSH)]·1.5(py)的合成、晶体结构及电化学性质研究

以DMF和吡啶为溶剂合成了镍的水杨醛缩水杨酰肼Schiff碱(SHSH)的配合物[Ni(py)₃(SHSH)]·1.5(py)(其中py代表吡啶)，成功培养出了单晶。通过UV、IR、元素分析和X射线衍射等进行了表征。中心镍离子与Schiff碱提供的2个氧原子和1个氮原子以及3个溶剂吡啶的氮原子参与了配位，形成了六配位的变形八面体构型，存在分子内氢键和分子间氢键。晶体属单斜晶系，空间群：P2₁/n。采用循环伏安法研究了其在吡啶和DMF溶液中的电化学性质。     

对硝基苯乙酮缩水杨酰肼Schiff碱的合成与晶体结构

合成了一种新的Schiff碱对硝基苯乙酮缩水杨酰肼,进行了红外光谱、紫外光谱和元素分析表征,并且测定了该化合物的晶体结构,该晶体属于单斜晶系,P2（1）／c空间群。晶胞参数a=1．6068（3）nm,b=1．1838（2）nm,c=0．729 01（15）nm,β=91．39（3）。     

HPLC Determination of Trace Hydrazine Levels in Phenelzine Sulfate Drug Substance

Abstract

An HPLC procedure for the estimation of trace hydrazine levels in phenelzine sulfate drug substance has been developed. The hydrazine is derivatized at ambient temperature with salicylaldehyde, and the salazine derivative is measured using short wavelength UV (209 nm). The salazine is separated from unreacted salicylaldehyde and other compounds using a mobile phase consisting of 60:40 acetonitrile-water. The mobile phase was pumped at a flow rate of 1.0 mL/min through a 150 mm × 4.6 mm i.d. reverse phase column (5 μm octadecylsilane, 30% carbon loading). The limit of detection of salazine produced when hydrazine sulfate reacts with salicylaldehyde in an analytical sample was found to be equivalent to 10 ppm of hydrazine (based upon 100 mg of phenelzine sulfate). Absorbance and hydrazine concentration are linear over the range of 10–1000 ppm of hydrazine, with an r² of 0.9998 (n=7) based on peak height. Five samples of phenelzine sulfate analyzed for hydrazine content with salicylaldehyde gave an interassay reproducibility of 2.1%.     

Influence of substituent effects on the coordination ability of salicylaldehyde Schiff bases

Abstract

The logK₁ was quantified by four parameters, metal ion radii R, metal ion charge Q, metal atom polarizability P, and Hammett constants σ of substituent, where logK₁ was the stability constant of complexes (179) involving 10 Schiff bases Sal-A-X (N-(5-chloro-4-6-dimethyl-benzylidene)-anilines) reacting with 18 metal ions. The effect of substituents on the coordination ability of Sal-A-X was systematically investigated, and an expression with good correlation was obtained. The result shows that the electronic effect of substituent X on the aniline ring has an important influence on the stability of the complex; its electron-donating effect enhances the stability of the complex, whereas its electron-withdrawing effect lowers the stability of the complex. The theoretical results provide a potential value for the design of coordination compounds with unique function and reactivity. Moreover, their coordination selectivity to specific metal-ions can also be evaluated according to Equation (2).     

A Novel and Facile Synthesis of 2‐(Benzofuran‐2‐yl)benzo[h]quinoline‐3‐carboxylic Acid Derivatives

A simple and concise approach for the synthesis of a series of new heterocyclic systems of 2‐(benzofuran‐2‐yl)benzo[h]quinoline‐3‐carboxylic acid derivatives ( 3a–3g ) is described. The synthetic strategy features the one‐pot reaction of ethyl 2‐(chloromethyl)benzo[h]quinoline‐3‐carboxylate ( 2 ) with various substituted salicylaldehydes as well as 2‐hydroxy‐1‐naphthaldehyde as a key step. The substrate 2 was prepared in good yield by a mild, efficient and direct reaction of 1‐naphthylamine ( 1 ) with Vilsmeier‐Haack reagent. The structures of all the new compounds were identified by spectral data and elemental analysis.     

An expedient synthesis of enantioenriched substituted (2-benzofuryl)arylcarbinols via tandem Rap-Stoermer and asymmetric transfer hydrogenation reactions

An expedient synthesis of enantioenriched substituted (benzofuran-yl)-aryl and heteroaryl carbinols, is described. A key feature of this protocol is synthesis of functionally varied benzofuran scaffolds via a Rap-Stoermer reaction/catalytic asymmetric transfer hydrogenation (ATH) using substituted salicylaldehyde and α-haloaryl, heteroaryl ketones.     

DABCO-Promoted Efficient and Convenient Synthesis of Benzofurans

An efficient and convenient synthesis of benzofurans has been described from phenacyl halides and o-hydroxy benzaldehyde in the presence of DABCO. The procedure is applicable for a variety of phenacyl halides and provide a variety of benzofurans. DABCO act as a base and as well as nucleophile.     

Efficient,High-Yield Protocol for the One-Pot Synthesis of Benzopyran Derivatives Catalyzed by p-TSA in Aqueous Media

A short and simple synthesis of benzopyran derivatives was accomplished in good to excellent yields by the reaction of salicylaldehyde with 1,3-cyclohexanediones in aqueous media catalyzed by para-toluenesulfonic acid. The structures were established by spectroscopic data and further confirmed by x-ray analysis. In addition, water was chosen as a green solvent.     

一种水杨醛异烟酰腙及其锌配位聚合物的合成、晶体结构和荧光性质

合成了一种酰腙类Schiff碱4-(二乙胺基)水杨醛异烟酰腙(H₂L·H₂O,1)并制备了它的锌配合物[Zn(L)(Phen)]_∞(2),用元素分析、红外光谱、紫外光谱、荧光光谱和X-射线单晶衍射分析等手段进行了表征.1的晶体属三斜晶系,P1空间群,晶胞参数a=0.71058(4)nm,b=1.0045(2)nm,c=1.3054(3)nm,α=97.383(11)°,β=102.989(12)°,γ=104.038(10)°,V=8.641(3)nm³,Z=2;分子间通过氢键作用形成一维链超分子体系.2的晶体属三方晶系,P3₁空间群,晶胞参数a=1.68654(12)nm,b=1.68654(12)nm,c=0.79656(12)nm,V=1.9622(5)nm³,Z=3;配合物结构基元由1个锌离子、1个邻菲咯啉和1个酰腙组成,通过吡啶环的桥联作用形成一种双螺旋状配位聚合物.1和2都能发射绿色荧光,最大发射波长分别为524和535nm.     

Solvent‐assisted planar structure of a stilbene‐based salicylhydrazone compound: crystal structure,solvent‐ and aggregation‐induced emission,and switchable luminescence colouration

A novel stilbene‐based salicylhydrazone compound {systematic name: (E)‐4,4′‐(ethene‐1,2‐diyl)bis[(N′E)‐N′‐(2‐hydroxybenzylidene)benzohydrazide] dimethyl sulfoxide disolvate, C₃₀H₂₄N₄O₄·2C₂H₆OS or L·2DMSO} was synthesized and characterized by single‐crystal X‐ray diffraction, powder X‐ray diffraction and luminescence spectroscopy. The title compound crystallizes in the monoclinic space group P2₁/c, with half a symmetry‐independent L molecule and one dimethyl sulfoxide (DMSO) solvent molecule in the asymmetric unit. The L molecule adopts an almost planar structure, with a small dihedral angle between the planes of the stilbene and salicylhydrazone groups. There are multiple π–π stacking interactions between adjacent L molecules. The DMSO solvent molecules act as proton donors and acceptors, forming hydrogen bonds of various strengths with the L molecules. In addition, the geometry optimization of a single molecule of L and its luminescence properties either in solution, as a solvated solid or as a desolvated solid were studied. The compound shows an aggregation‐induced emission (AIE) effect and exhibits switchable luminescence colouration in the solid state by the simple removal or re‐addition of the DMSO solvent.