基地建设经验交流

南京大学化学化工学院于1991年被国家教委批准为首批国家基础科学研究和教学人才培养基地."基地方案的制定和实施"于1997年获国家教委优秀教学成果二等奖,并于1998年在国家自然科学基金委组织的中期评估中获得优秀基地的称号,1999年又以优异成绩顺利通过了教育部组织的基地挂牌验收.     

脱羧氯雷他定的合成

脱羧氯雷他定 (ＤＣＬ)是一种有效的非镇定性抗组织胺 ,对过敏性鼻炎 ,糖尿病、咳嗽、普通感冒、流行性感冒、关节痛及其它不适症状都有很好的疗效[1～2 ] 。它克服了氯雷他定、酮康唑、红霉素、伊曲康唑等易引发黑色素瘤、纤维肉瘤、胃刺激、肥胖症、心律失调、传导紊乱等症状的缺点。且它的使用剂量只有氯雷他定的十分之一 ,有很好的市场前景和实际应用价值。ＭａｒｋＷ .Ｈｏｌｌａｄａｙｅｔａｌ[3] 在水溶液中由酸、碱催化得到了脱羧氯雷他定 ,但无具体操作和反应结果报道。Ａ .Ｋ .ＧｕｎｎａｒＡｂｅｒｇ[1] 直接用ＫＯＨ在绝对无水…     

手性双氨基醇-Et2Zn催化的不对称直接羟醛缩合反应

以1,3-二溴丙酮和(2'S)-(二苯基羟甲基)-四氢吡咯为原料,合成了两种新型手性氨基醇1,3-双[(2'S)-(二苯基羟甲基)-1-四氢吡咯基]丙酮(3)和1,3-双[(2'S)-(二苯基羟甲基)-1-四氢吡咯基]-2-丙醇(4),总产率分别为39%和35%.手性双氨基醇3-/4-Et2Zn可催化未修饰醛、酮的不对称直接羟醛缩合反应,对映体过量最高9%.     

Fe和Co催化的碳-碳偶联反应的最新进展

作为廉价而且低毒的金属, Fe和Co是发展催化剂的理想元素. 同时由于Fe和Co有着多种氧化还原价态, 它们的催化化学应该具有极其丰富的内容. 然而由于种种原因, Fe和Co的催化剂很少得到有机化学家的关注. 直到最近几年, 人们才发现Fe和Co的催化剂可以很好地催化碳-碳偶联反应. 综述了Fe和Co催化碳-碳偶联反应的条件、产率和选择性; 探讨了这些新奇反应的可能机理; 并介绍了这些反应在复杂化合物合成中的应用.     

Electrocatalysis of the SiC Particle‐Modified Glassy Carbon Electrode for the Oxidation of Adrenaline

The electrocatalytic properties of the SiC particle‐modified glassy carbon electrode (MGC) for adrenaline oxidation were studied by cyclic voltammetry (CV), double‐potential step chronocoulometry (DPSCC), and electrochemical impedance spectroscopy (EIS) techniques in McIlvaine buffer solution. It was shown that the electrode modified with SiC particles markedly displayed an electrocatalytic effect on the process of the electrochemical reaction of adrenaline, i.e., the activity and the reversibility of the MGC electrode has been significantly improved. This was attributed to the adsorption effect of the electroactive adrenaline molecules on the MGC electrode surface.     

Novel Synthesis of Dihydroquinoxalinylpyridazine Derivatives

Methylquinoxaline derivative 1 undergoes bromination to give bromomethyl quinoxaline 2 , which could be transferred to cyanomethyl quinoxaline 3 . The latter compound 3 readily coupled with arene diazonium salts to give hydrazone derivatives 5a‐c . Compounds 5a,b reacted with active methylene reagents to give the target ring system, quinoxalinylpyridazine derivatives 8a‐c . Compound 1 reacted with DMFDMA to give the enamine derivative 9 , which coupled with arene diazonium salts to give the aldehydic hydrazone derivatives 10a‐c . Compound 10 reacted with active methylene compounds to give quinoxalinylpyridazine derivatives. UV characterization of some of the prepared compounds was reported.     

电解沉积压电频移分析的理论与验证

提出了控制电位电解和恒电流电解两类电解沉积的压电频移分析法测定的理论公式,用实验结果验证了它的正确性.     

Electric conductivity in a fibrous porous medium with thin but polarized double layers

The electric conduction in the fibrous medium constructed by a homogeneous array of parallel, identical, charged, circular cylinders having an arbitrary zeta potential filled with the solution of a symmetrically charged electrolyte is analytically examined. The thickness of the electric double layers surrounding the dielectric cylinders is assumed to be small relative to the radius of each cylinder and to the gap width between two neighboring cylinders, but the polarization of the mobile ions in the diffuse layers is allowed. The effect of interactions among individual cylinders is taken into explicit account by employing a unit cell model. The appropriate equations of conservation of electrochemical potential energies of ionic species are solved for each cell, in which a cylinder is envisaged to be surrounded by a coaxial cylindrical shell of the fluid solution. Analytical expressions for the effective electric conductivity are obtained in closed forms as functions of the porosity of the fiber matrix and other characteristics of the porous system. Comparisons of the results of the cell model with different conditions at the outer boundary of the cell are made. Under an otherwise identical condition, the electric conductivity in a porous medium composed of an array of parallel cylinders in the transverse direction is smaller than that of a suspension of spheres. The effect of interactions among the cylinders or spheres on the effective conductivity can be quite significant under appropriate conditions.     

[Cu(C8H4F3O2S)2(C12H8N2)]·C3H6O的合成及其晶体结构

标题配合物 [Cu(C8H4 F3O2 S) 2 (C12 H8N2 ) ]·C3H6 O属于三斜晶系 ,空间群为P1,并测得如下晶胞参数a =10 .5 77(3) ,b =15 .72 2 (4) ,c =10 .133(2 ) ,α =94 .5 3(2 ) ,β =10 0 .81(2 ) ,γ =96 .18(2 )° ,V =16 37.0 3 3,Z =2 ,Mr =74 4.18,Dx =1.5 1× 10 6 g·m- 3,F(0 0 0 ) =5 2 6 ,μ =8 2 4cm- 1,最终偏差因子为R =0 .0 83,Rw=0 .0 74。Cu(II)与 2个 4 ,4 ,4 三氟 1 (2 噻吩基 )丁二酮 1,3中的四个氧原子和菲咯啉中的两个氮原子 ,组成了一个畸变的八面体构型。     

Determination of Naphthalenesulfonate Isomers in Industrial Effluents and River Water by Solid‐Phase Extraction and Capillary Zone Electrophoresis

This work presents a method to separate polar naphthalenesulfonate (NS) isomers by capillary zone electrophoresis (CZE) with ultraviolet detection in industrial effluents and river water samples. The method involves extraction of samples by a polystyrene‐divinylbenzene copolymer (PS‐DVB) solid‐phase extraction (SPE) cartridge. The most effective CZE separation conditions were obtained in 20 mM borate buffer with 30% acetonitrile at pH 9.0 and 30 °C. The method proposed herein provides a high precision and sensitivity for NS isomers, to quantitation at ≤ 1.0 μg/L in 200 mL of the water samples. Recovery of the NS isomers in spiked water samples ranged from 73% to 87% while RSD ranging from 5.6 to 9.7%. The analysis of industrial effluents and river water samples was performed and naphthalene‐2‐sulfonate was found as a major pollutant. The difficulties in quantitating and identifying analytes in complex environmental samples can be resolved by using an internal standard response factor to calculate concentrations and relative migration times for peak confirmation.