5,7-二甲氧基-4-甲基苯酞和5,7-二羟基-4-甲基苯酞的新合成方法

以3,5-二甲氧基苯甲醇为起始原料, 经过五步反应, 合成了5,7-二甲氧基-4-甲基苯酞和5,7-二羟基-4-甲基苯酞这两个用于合成霉酚酸的重要中间体, 产率分别达到80%和72%. 6-氯甲基-2,4-二甲氧基苯甲醛经过亚氯酸钠氧化成酸的同时发生内酯化反应生成5,7-二甲氧基苯酞是最关键的一步.     

取代二氢异喹啉基苯基甲基酮的合成新方法

以3,4-二甲氧基苯乙酸为原料,经氯化亚砜酰氯化、3,4-二甲氧基苯乙胺氨解得到了N-(3,4-二甲氧基苯乙基)-2-(3,4-二甲氧基苯基)乙酰胺,经Bischler-Napieraski反应环化同时氧化,合成了Lamellarin重要中间体(6,7-二甲氧基-3,4-二氢异喹啉-1-基)(3,4-二甲氧基苯基)甲基酮,优化了环化的反应条件,其总收率为56%。此方法未见文献报道。产物用1H NMR、13C NMR、MS、IR进行了表征。     

3,4-二甲氧基-6-氨基苯甲醛的合成

以藜芦醛为原料合成4,5-二甲氧基-2-硝基苯甲醛,经铁粉还原后高产率地得到了3,4-二甲氧基-6-氨基苯甲醛。     

天然产物5,7-二甲氧基-4′-羟基异黄酮的合成

以4-羟基苯乙酸和3,5-二甲氧基苯酚为原料,通过一条包括苄基化、酰氯化、酯化、氢化、Fries重排、以及Vilsmeier-Haack反应等6步反应的路线合成了天然产物5,7-二甲氧基-4′-羟基异黄酮,目标产物的总收率为33%.利用1HNMR、13C NMR及元素分析确证了化合物的结构.     

2-甲氧基-4-氯苯甲酸的合成新方法

以间氯苯酚为原料,经乙酰化、Fries重排、O-甲基化和氧化反应合成了2-甲氧基-4-氯苯甲酸,总收率54.1%,纯度98.2%.     

5-甲氧基-2-苯基-2, 3-二氢苯并呋喃的制备——介绍一个大学综合化学实验

介绍了一个大学综合化学实验。该实验以对甲氧基苯酚和苯乙烯为原料,六氟异丙醇为溶剂,2,3-二氯-5,6-二氰基-1,4-苯醌为氧化剂,室温合成5-甲氧基-2-苯基-2,3-二氢苯并呋喃,并用IR、1H NMR、13C NMR和HRMS对产物结构进行表征。本实验有益于激发学生的科研兴趣和探索精神,训练学生的综合实验操作技能和分析能力,培养学生的创新思维和科研能力。     

2-甲磺酰基-4,6-二甲氧基嘧啶的简便合成

以2-硫代巴比妥酸为原料,在相转移催化剂的作用下,超声促进与硫酸二甲酯反应,得到2-甲硫基-4,6-二甲氧基嘧啶,再经次氯酸钠氧化得到2-甲磺酰基-4,6-二甲氧基嘧啶,总收率63％。     

一种有效合成5,7-二甲氧基-1-茚酮的方法

成功开发一种由容易得到的2-(3,5-二甲氧基苄基)丙二酸二乙酯为原料合成5,7-二甲氧基1-茚酮的有效新方法。将原料溶解于甲磺酸中,加热到100℃反应2 h收率可以达到95%。本反应所需原料廉价、后处理简单、对设备要求不高,适用于工业化生产。另外,文中还提出了该反应可能的反应机理。     

(S)-3-(3,4-二甲氧基苯基)-2-甲基丙氨酸衍生的手性咪唑啉酮催化剂合成新方法

以(S)-3-(3,4-二甲氧基苯基)-2-甲基丙氨酸盐酸盐为原料,针对其合成咪唑啉酮催化剂过程中反应条件苛刻和反应时间长等问题,重新设计了一条合成路线,并考察了温度、原料摩尔比和反应时间等对合成收率的影响。新合成路线中,合成关键中间体(S)-3-(3,4-二甲氧基苯基)-2-甲基丙氨酸甲酰胺7的反应时间由9 d缩短至7 h,不需剧毒的NaCN催化,收率达到98%。     

2-羟基-3,4,6-三甲氧基查尔酮的合成

本文开发了一种天然产物2-羟基-3,4,6-三甲氧基查尔酮(1)的十克级规模快速合成方法。通过改良合成2-羟基-3,4,6-三甲氧基苯甲醛(7)的甲基化和甲酰化条件,将7的合成总收率从文献报道的22%提高至68%。并以7为原料在乙腈为溶剂、80℃加热的条件下通过Wittig反应在50mmol规模以85%的收率合成了产物1。     

微量元素对固态锡在持续升温时氧化过程的影响

用DTA、TG研究了不同粒度纯Sn和含微量Ga、S、Cu时的Sn在20℃·min-1的持续升温过程中的氧化过程,测定了升温过程中间产物的XRD图.结果表明,随着粒度增大,Sn开始氧化的温度提高.添加0.1%的Ga提高了锡的氧化稳定性,表面生成一层SnO;添加微量Cu对Sn的氧化影响很小;添加0.1%的S时,氧化稳定性降低.氧化过程中,除添加Ga者外,其它无中间产物SnO生成.     

电化学和石英晶体微天平研究2-巯基苯并咪唑的电化学氧化反应

应用循环伏安研究水相中２－巯基苯并咪唑的电化学氧化过程,考察了ｐＨ值、浓度等的影响,并应用电化学石英晶体天平（ＥＱＣＭ）监测了此氧化成膜的过程。结果表明此反应为一电子过程。结合表面光电子能谱（ＸＰＳ）对此氧化膜进行了初步表征。     

On the Reactivity of Silver Electrodes in a Chlorine Radiofrequency Plasma — Plasma Oxidation vs. Thermal Oxidation

The plasma‐electrochemical growth of an ion‐conducting film by the oxidation of a metal in an electronegative plasma is investigated and compared with results from thermal oxidation. As model system we studied the oxidation kinetics of silver electrodes in a Cl₂ rf plasma. The electrochemical control of the reaction by external currents through the product layer using the plasma as a fluid electrode was achieved. Both potentiostatic and galvanostatic control of the reaction was applied. The morphology of the product layer and its temporal evolution was investigated using SEM. A formation of silver chloride surface patterns in the oxidation process takes place if a simple stability criterion is not fulfilled. Specific surface morphologies were found under different experimental conditions. The morphology of the product layer is influenced by the external electric current and the substrate temperature. The influence of the plasma phase on the thermodynamics and kinetics of the oxidation process is discussed. The role of excited plasma species, the electrical charging of the surface and radiation from the plasma are taken into account.     

Electrochemical Oxidation of Berberine and of Its Oxidation Products at a Glassy Carbon Electrode

The electrochemical behavior of berberine, an isoquinoline plant alkaloid with a wide spectrum of physiological effects, was studied at a glassy carbon electrode using cyclic, differential pulse and square‐wave voltammetry. The oxidation of berberine is a quasireversible, diffusion‐controlled process and occurred in a cascade mechanism with the formation of several oxidation products. The diffusion coefficient of berberine was calculated from cyclic voltammetry studies to be D=1.69×10^?6 cm² s^?1. The oxidation process of berberine is also pH dependent and the number of electrons and protons transferred was determined using differential pulse voltammetry. The formation of several oxidation products that adsorbed at the glassy carbon electrode surface was observed and their electrochemical behavior characterized. A mechanism for the oxidation of berberine at a glassy carbon electrode was proposed.     

Experimental assessment of electrochemical processes in the remediation of atrazine contaminated soils

The electrochemical oxidation of an atrazine solution obtained from a flushing treatment of a contaminated soil was investigated. The influence of ethanol on atrazine oxidation was studied. Results show that the electrogenerated Fenton's reagent provides a complete degradation of atrazine and its main chlorinated by-products via N-dehalkylation and dechlorination. This process therefore presents an effective alternative to the chemical oxidation treatment which necessarily needs a further biological state.     

Catalytic properties of the carbides of transition metals in oxidation reactions

It was shown that the carbides of transition metals are effective catalysts of oxidation reactions on account of their metal-like nature, combined with their high chemical and thermal stability. The results from systematic investigations into the catalytic characteristics of the carbides in the oxidation of hydrogen, carbon monoxide, and ammonia and in the oxidative coupling of methane (OCM) are examined. The first two reactions are total oxidation processes, and the oxidation of ammonia is a selective oxidation process. The oxidative coupling of methane is a heterogeneous-homogeneous process and represents a prospective method for the direct transformation of methane into higher hydrocarbons. L. V. Pisarzhevskii Institute of Physical Chemistry, National Academy of Sciences of Ukraine, 31 Prospekt Nauki, Kiev 252039, Ukraine. Translated from Teoreticheskaya i éksperimental'naya Khimiya, Vol. 34, No. 5, pp. 265–281, September–October, 1998.     

流光放电等离子体液相氧化亚硫酸铵

在氨-硫铵法烟气脱硫中, 一个关键环节是将副产物的四价硫S(IV)氧化为六价硫S(VI). 采用可规模化的流光放电液相氧化技术, 通过交直流叠加(AC/DC)电源, 激发气体放电产生等离子体对氨法脱硫高浓度的亚硫酸铵进行氧化. 实验测量了该氧化过程与溶液浓度、放电功率密度、溶液pH值、温度以及传质效率因子等各种参数的关系. 研究表明, 在亚硫酸铵摩尔浓度为3 mol·L-1时, 可以获得有实用价值的反应速率, 摩尔能耗减低到50 Wh·mol-1以下, 显示出很好的应用前景.     

Electrocatalytic Oxidation of Hypophosphite on Nickel Electrode ──In Situ UV-Vis Spectroscopic study

ThefactthathypophosphiteisoneofthemostwidelyusedreducingagentsintheNielectrolessdepositionhasstimulatedthestudyofanodicoxidationofhypophosphiteonnicked-ic.Thisanodicreaction,whichisimportantfortheunderstandingoftheNielectrolessdepositionmechanism,isexpectedtobeoneoftheimportantreactionsintheNi-electrolessprocess.Recently,theroleandoxidationmechanismofhypophosphiteinelectrolessdepositionofNi-Palloyhavebeenstudiedindetailusingtheprobebeamdeflection',electrochemistryandinsituIR',lo.However,som…     

2,2,6,6-四甲基哌啶氧自由基/Ca(ClO)2催化氧化甲基葡糖苷制备葡醛酸

采用2,2,6,6-四甲基哌啶氧自由基/Ca(ClO)2体系选择氧化甲基葡萄糖苷(简称甲苷)合成了葡萄糖甲苷酸盐,再用硫酸酸解葡萄糖甲苷酸盐,得到葡萄糖醛酸和副产物硫酸钙。考察了氧化工艺条件对葡萄糖醛酸收率的影响;用pH计监控反应过程,反应中间体和终产物用UV和HPLC检测。结果表明,该体系对甲苷伯羟基的氧化具有较好的催化活性和反应选择性,葡萄糖醛酸收率达到92%,且金属离子易于去除。和传统的淀粉HNO3氧化法工艺相比,该方法具有资源节约、环境友好的特点。     

甲酸在铂电极上吸附氧化机理研究

用时间分辨石英晶体微天平（Ｔｉｍｅ－ｒｅｓｏｌｖｅｄ ＥＱＣＭ）、循环伏安法及电化学阶跃技术,研究了铂电极上甲酸的吸附氧化过程。结果表明,在活性吸附氧化过程中,甲酸吸附后迅速失去一个电子形成ＣＯＯＨａｄ单分子层,在阶跃电势计时电流图上得到一个氧化电流峰及ＥＱＣＭ图上一个相应的质量增加,随后的ＣＯＯＨａｄ氧化是一个速率较慢的过程,当它的吸附达到稳成以后,甲酸氧化反应在计时电流图上表现为稳态小电流及相