芳香酮曼尼希碱酸化缓蚀剂的合成及复配研究

以37%的甲醛溶液、苯乙酮和二乙胺为原料,合成一种新型曼尼希碱盐酸酸化缓蚀剂,并对其进行复配研究。结果表明,最佳合成条件为:二乙胺、37%甲醛溶液和苯乙酮的摩尔比为2:2:1,反应时间8 h,反应温度80℃,pH值为4;钨酸钠和缓蚀剂有着很好的正协同效应,碘化钾与其有负协同效应。     

Synthesis,characterization, spectral and antifungal properties of some 5-Substituted-1,3,4-oxadiazole-2-thiones and their mannich bases

A series of 5-substituted aryloxymethyl-1,3,4-oxadiazole-2-thione ( 3a–e ) and their Mannich bases 4–8 are synthesized and subjected to fungitoxic screening. The structures of these compounds are established on the basis of elemental analysis ¹H-n.m.r. and mass spectral data. The mass spectral fragmentation pathways of these compounds are discussed.     

4-氨基安替比林双席夫碱的合成与表征

利用水杨醛和4-氨基安替比林为原料,合成了两个新型双席夫碱.目标产物结构经 ~1HNMR、IR和MS等表征.     

萘乙酰基吡唑啉酮及其席夫碱的合成与表征

在非水溶剂中合成出一种未见报道的新型酰基吡唑啉酮试剂:1-苯基-3-甲基-4-萘乙酰基-吡唑啉酮-5(PMNAP)及其3 种席夫碱化合物.通过元素分析、红外光谱、质谱和核磁共振氢谱对其进行了结构表征.表征结果显示:PMNAP以酮式结构存在,形成席夫碱后的3种化合物均以酮式和烯醇式两种结构并存.     

4-氨基安替比林席夫碱的合成与表征

用4-氨基安替比林与3-甲酰基色酮、肉桂醛、茴香醛反应分别合成了3种新的席夫碱化合物。利用元素分析、红外光谱和核磁共振氢谱确认了它们的结构。     

两种新含硫席夫碱的合成与表征

报道了两种新含硫席夫碱－维生素Ｋ３单缩二氨基硫脲和丙酮酸二缩二氨基硫脲的合成，这两种化合物至今尚未文献报道。通过元素分析，质谱，红外光谱和核磁共振氢谱对两种化合物的结构进行了表征。     

含硫双Schiff碱及其金属配合物的合成、表征与生物活性研究

合成了茚三酮-1,3-双缩肼基二硫代甲酸苄酯(HL1),茚三酮-1,3-双缩氨基硫脲(HL2)两种含硫双Schiff碱及它们的铜、钴金属等配合物,通过元素分析、红外光谱、紫外-可见光谱、差热和摩尔电导等测试对其进行了表征,并测试了双Schiff碱配体与金属配合物对大肠杆菌、枯草芽孢杆菌的抑菌活性。     

Synthesis and characterization of copper(I) complexes from triphenylphosphine and isatin Schiff bases of semi- and thiosemicarbazide

The reaction of isatin-3-thiosemicarbazone (ITC, 1) or isatin-3-semicarbazone (ISC, 2) with nitrato bis(triphenylphosphine)copper(I) gave the four coordinate copper(I) complexes [Cu(PPh₃)₂(ITC)]NO₃ (3) and [Cu(PPh₃)₂(ISC)]NO₃ (4). The synthesized complexes were characterized by FT-IR, UV–VIS, Raman and elemental analysis. The crystal structure of 3 was investigated by single crystal X-ray diffraction. The ITC coordinates to the copper(I) ion in a bidentate fashion via the N(imine) and S atoms which along with two triphenylphosphine ligands form a tetracoordinate complex. The complex has a distorted tetrahedral coordination environment. Crystal data at 150.0 K: space group P2₁/c with a=12.5777(4), b=15.2062(5), c=21.9057(7) Å, β=95.628(3)^o, Z=4, R ₁=0.049.

     

N-(1-萘基)-4-烷氧基苯甲亚胺席夫碱的合成与表征

以对羟基苯甲醛与卤代烃CnH2n 1X(n=2,4,8,14,16)为原料,通过Williamson反应合成对烷氧基苯甲醛中间体,再与α-萘胺缩合得到5个新的含萘基席夫碱化合物.通过对n=8的席夫碱缩合反应进行L9(34)正交试验,得到缩合反应最佳条件:无水乙醇为溶剂,投料物质的量比为1∶1,温度为65 ℃,时间为8 h.中间体及席夫碱系列化合物的结构用FT-IR、1HNMR进行了表征,并利用DSC考察了柔性链碳原子数对席夫碱相态变化的影响.     

Synthesis and application of polycarbosilane supported manganese ions as catalyst in mannich reaction

Polycarbosilane (PCS) with highly crosslinked structure and high surface area was synthesized by the polycondensation reaction between trimethoxyvinylsilane and trichloromethylsilane. The reaction was conducted in the presence of sodium metal. Manganese ion was supported on PCS. The immobilization of transition metal ions to polymer support leads to a number of advantages over homogeneous catalyst, viz easy product recovery, increased selectivity, etc. The catalytic activity of PCS supported manganese ion was studied by considering three‐component Mannich reaction. Reaction with diverse sets of aldehydes, amines, and ketones was examined. PCS‐supported manganese ion catalyst has been prepared for the first time and used successfully in Mannich reaction. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Synthesis and characterization of polythioetheramide from allylamine

Summary A novel polythioetheramide was synthesized from allylamine and 3-mercaptopropionic acid with a free-radical initiator. The thioether and amide linkages are formed from the free-radical addition of -SH group to double bond and the condensation between -NH₂ and -COOH, respectively. The free-radical addition gives almost exclusively anti-Markovnikov product. The resulting polymer has a glass-transition temperature of 8.5 °C and a melting point of 145 °C. Though the introduction of the thioether linkages increases flexibility, the polymer retains good solvent resistance. Received: 1 June 1998/Revised version: 24 August 1998/Accepted: 27 August 1998     

New organic polymers,I. Synthesis and characterization of poly Schiff bases from benzidine-3,3′-dicarboxylic acid

Thermally stable and semiconducting polymers are synthesized by condensing benzidine-3,3′-dicarboxylic acid (BDC), with dicarbonyl compounds like glyoxal, cyclohexane-1,4-dione, 4,4′-diacetyl diphenyl ether and benzil under different experimental conditions. These poly Schiff bases are insoluble in common organic solvents. They are characterized by IR- and viscosity studies, thermal analysis, and the study of electrical properties at various temperatures. Variation of the electrical conductivity, σ, with temperature was found to confirm with the empirical relation:      

Synthesis,characterization and catalytic activities of ruthenium complexes containing triphenylphosphine/triphenylarsine and tetradentate Schiff bases

Ruthenium(II) complexes of the type [Ru(CO)(B)(L)] (B=AsPh₃, pyridine, piperidine or morpholine; L=dianion of tetradentate Schiff bases) have been synthesized and characterized by physico-chemical methods. These complexes are found to be effective catalysts in the oxidation of primary and secondary alcohols using N-methylmorpholine-N-oxide as oxidant. The catalytic activity of these triphenylarsine complexes have been compared with that of triphenylphosphine complexes and with similar ruthenium(III) complexes. The formation of high valent Ruⁿ⁺²O species as catalytic intermediate is proposed for the catalytic processes.     

吡啶碱的合成及应用前景

吡啶碱广泛应用于医药、农药、香料、橡胶和染料的生产。吡啶碱的生产方法主要有两种:一是从煤焦油中提取;二是从氨和甲醛、乙醛的合成过程中获得。欧盟、美国、日本是主要的生产国,主要采用合成法生产。2000年底,比利时的Reilly公司和中国南通醋酸厂合作建立了1.1万t的吡啶系列产品生产厂,填补了国内合成吡啶的空白。     

Synthesis and characterization of polymers derived from selenophene

The synthesis of poly(2,5‐selenophen‐oxo‐1,4‐phenylen‐selenide‐1,4‐phenylene‐oxo) (I) and poly(2,5‐selenophen‐oxo‐1,4‐phenylen‐diselenide‐1,4‐phenylen‐oxo) (II) by reaction of 2,5‐bis(1,4‐bromo‐phenylen‐oxo‐)‐selenophene with sodium selenide or diselenide, respectively, using dimethylformamide as solvent, is described. Both monomers and polymers were characterized by elemental analysis, melting point, and FTIR spectroscopy. Polymers I and II were doped with iodine and SbF₅ and characterized by SEM and XPS. Also, the conductivity and the T_g values were determined. For both polymers the best doping agent was iodine, although polymer II always presented higher conductivity, reaching values of about 6 · 10^?9 S · cm^?1. The T_g values suggest a likely crosslinking of the chains in polymer II when doped with SbF₅. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 2019–2026, 2001     

基于催化氨化反应由生物质基小分子合成腈类和吡啶碱

基于催化氨化反应以生物质基小分子合成腈类、吡啶碱等含氮化学品,不但可减少生产此类产品对化石资源的依赖,还可促进生物质基小分子产业的可持续发展。本文结合本文作者课题组的研究成果总结了近年来在乙醇、甘油催化氨化合成腈类、吡啶碱的最新研究进展。其中,乙醇可高收率地生产乙腈,也可在脱氢、适宜酸性催化剂催化下生成吡啶碱。甘油在适宜催化剂上既可以通过一步法也可以通过两步法转化为腈类和吡啶碱,其中催化剂适宜的酸性、较强的加氢-脱氢性能以及较大的比表面是决定生成何种目标产物的关键。采用两步法比一步法由甘油合成腈类和吡啶碱的收率明显提高。发现催化剂在使用中逐渐失活,而催化剂失活主要是由于亚胺中间体在催化剂酸中心的不可逆吸附,从而生成积炭所致。失活催化剂经高温有氧煅烧去除积炭可恢复其大部分活性。     

Chelating resins. III. Synthesis,characterization, and capacity studies of formaldehyde-condensed phenolic schiff bases derived from 1,2-diamines and hydroxy benzaldehydes

Schiff bases of hydroxy benzaldehydes with aliphatic and aromatic 1,2-diamines were re-sinified in HCHO in alkaline media. These resins were found to form complexes readily with Cu(II), Co(II), and Ni(II). The materials were characterized by infrared, ¹H-NMR, UV-visible (UV-vis) spectral studies, and thermogravimetric analyses. The phenolic oxygen and the azomethene nitrogen were the ligating sites, one or more lattice positions in polychelates being occupied by water molecules. ¹H-NMR provided evidence for bridging methylene and terminal methylol groups. The UV-vis spectra showed weak absorptions in the d—d transition range. Capacity studies of the resins indicated metal loading up to 70% at room temperature in an appropriate pH of the salt solutions. The effects of contact time, particle size of the sorbents, resin quantity, and pH on the adsorption characteristics were studied. In the pH range 3-8, the resins derived from the structurally rigid Schiff bases exhibited higher capacity for the metal ions than the resins derived from structurally flexible Schiff bases. Kinetic parameters computed from the thermogravimetric data indicated the resins to be more stable than the corresponding polychelates. © 1996 John Wiley & Sons, Inc.     

Synthesis and characterization of resins from urea and acrolein

The reactions of urea with acrolein in neutral and acidic media were studied by means of ¹H- and ¹³C-NMR spectroscopy. The addition of aldehyde groups to urea seems to be the first step of the reaction. In the second step in neutral medium the groups and the double bonds react with the amide groups. In the acidic medium the condensation of as second step was dominant. In the further course of the reaction highly crosslinked resins are formed which are insoluble and unmeltable. Chemical shifts of individual compounds are given. On the basis of these data, it was possible to set up tentative reaction schemes. The determination of the concentrations of reaction products as functions of reaction time allowed to establish the kinetics of individual reactions.     

二茂铁席夫碱类衍生物的合成

以二茂铁,取代胺为原料,经甲酰化、缩合反应,合成了七个具有大π共轭体系的二茂铁席夫碱有机金属三阶非线性光学材料。分析合成反应过程,优化反应条件,得出以碱性Al2O3为催化剂,在回流温度下,以二甲苯为溶剂,产物收率为59.1%。比较了不同的取代胺对反应收率的影响,得出胺的碱性越强,反应收率越高。所有化合物均由核磁共振（1HNMR）、紫外（UV）、质谱(MS)等表征了结构。方法简单、可行。