锌-丙酸铵还原体系用于氢化偶氮苯的合成

选用锌粉和镁粉与不同饱和铵盐（草酸铵、丙酸铵和苯甲酸铵）水溶液组成还原体系,由偶氮苯制备氢化偶氮苯,根据反应时间及结果选取锌一饱和丙酸铵水溶液为最佳还原体系。在反应温度25℃时,研究了锌一饱和丙酸铵水溶液还原体系还原偶氮苯反应,考察了偶氮苯与锌粉物质的量比、饱和丙酸铵水溶液的用量对氢化偶氮苯收率的影响。实验结果表明：偶...     

锌—柠檬酸氢二铵还原体系用于氢化偶氮苯的合成

采用锌-柠檬酸氢二铵溶液还原体系,以偶氮苯为原料合成出氢化偶氮苯.合成反应的最佳反应条件：当偶氮苯用量是0.625 mmol时,偶氮苯与锌的物质的量之比为1：5,0.2 g/mL柠檬酸氢二铵溶液用量5.0 mL,室温,时间约3 min,平均收率90.63％.     

两种Zn-饱和铵盐还原体系用于氢化偶氮苯的合成

采用Zn-饱和甲酸铵溶液、Zn-饱和苯甲酸铵溶液还原体系,从偶氮苯制备氢化偶氮苯。Zn-饱和甲酸铵溶液还原体系的优化反应条件为:偶氮苯/锌物质的量比为1∶3(偶氮苯2.5 mmol),饱和甲酸铵溶液1.0 mL,反应时间5 min,产率87.5%。Zn-饱和苯甲酸铵溶液还原体系的优化反应条件为:偶氮苯/锌物质的量比为1∶3(偶氮苯0.625 mmol),饱和苯甲酸铵溶液2.0 mL,反应时间3 min,产率86.4%。     

甲醛还原法制备2,2′-二氯氢化偶氮苯

2,2'-二氯氢化偶氮苯（DHB）主要用于制备3,3'-二氯联苯胺（DCB）.DCB是重要的有机颜料中间体。     

离子交换膜法合成2,2′-二氯氢化偶氮苯

应用离子交换膜法电解邻氯硝基苯合成2,2′-二氯氢化偶氮苯.讨论了电极活化条件、电流密度、电解液温度等因素对电解还原反应的影响.结果表明:在反应温度t=80℃,阴极、阳极电解液分别为10%和30%(by m ass)的NaOH溶液,电流密度4.2A/dm2条件下电解,电流效率最高,可达73%,收率为83%.     

Pd/C催化硝基苯氢化制氢化偶氮苯的研究

在碱性甲醇溶液中 ,硝基苯在Pd/C催化作用下能高产率地选择性氢化还原为氢化偶氮苯 ,2h转化率达10 0 % ,产品收率 98.5 %以上 .通过XRD初步分析了催化作用原理 ,并提出了可能的反应机理     

甲醛还原法制备2,2'-二氯氢化偶氮苯

二氯氧化偶氮苯;二氯联苯胺;还原过程;甲醛还原法制备2;2'-二氯氢化偶氮苯     

2-羟基-3-羧基-5-磺酸基苯重氮氨基偶氮苯分光光度法测定微量锌

1引言本重氮氨基偶氮苯类试剂是分析性能优良的显色剂，2-羟基-3-羧基-5-磺酸基苯重氮氨基偶氮苯（HCSDAA）是其中新近合成的一种。我们已研究了其用于微量汞、铊、铜的分光光度测定和汞、铜的流动注射分析。本文发现，HCSDAA也是锌的高灵敏显色剂，据此提出的测定锌的方法灵敏、简便、选择性好，可不经预分离或使用掩蔽剂直接测定人发和锌强化营养盐中微量锌．2实验方法移取适量锌标准溶液于10mL比色管中，依次加入1％乳化剂OP＄液1。mL，0．04％HCSDAA乙醇溶液亚．8mL、0．05mol／L硼砂一Na0H缓冲溶液（pH11．0）2．5mL，用水…     

新显色剂4,4′-二偶氮苯重氮氨基偶氮苯测定水中微量锌的研究

本文报告在四硼酸钠体系中和Triton X-100存在下,锌与新显色剂4,4′-二偶氮苯重氮氨基偶氮苯有灵敏的显色反应。红色络合物在525nm处摩尔吸光系数为1.63×10~5L·mol~(-1)·cm~(-1),并研究了测定锌的各种条件和40余种共存离子对测定的影响。     

偶氮苯镁配合物的合成和结构

金属镁具有较强的还原性,可以促进加氢还原、亚砜脱硫、二元醇消除、混合醚制备等反应[1],在有机合成化学上是一种常用且有效的催化剂或反应试剂.但是迄今为止,除对格氏反应研究比较透彻外,金属镁和有机底物分子的基元反应研究报道极少,这导致了金属镁在很多有机反应中的催化作用机理往往不很清楚.     

Reactions of hydrazobenzene and tetranitromethane with nitroxyl radicals

The values of isotropic HFS constantsa _N were obtained for nitroxyl radicals (NR) of the piperidine series in hexane and water. The interrelation between rate constants for NR reduction and oxidation reactions, isotropic HFS constantsa _N, inductive constants of the piperidine substituents, and electrochemical characteristics of NR were found. The dependence of the rate constants for the reduction of NR by hydrazobenzene (HB) and its oxidation by tetranitromethane (TNM) upon the Hammett type inductive constants _EPR, obtained using HFS constantsa _N as the basis, was analyzed. The solvent effect on the reduction and oxidation reaction rate constants, the kinetic isotopic effect of the reduction reaction for a number of NR-HB systems, and alternative reaction mechanisms are considered.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1074–1079, June, 1993.     

乙酸4-氯甲基苯酯的改进合成

以廉价的4-羟基苯甲醛为原料，在温和条件下先后经硼氢化钠还原和与乙酰氯反应，合成了乙酸4-氯甲基苯酯，其结构经元素分析，IR，1H NMR和13C NMR确证。     

4-氨基丁醇的高效合成方法

以2, 3-二氢呋喃为原料,先用酸性水溶液处理,得到的粗品再直接与盐酸羟胺发生反应,得到4-羟基丁基肟,再与还原试剂发生还原反应,最终高效得到4-氨基丁醇产品。此合成方法步骤短且易操作,产率高,可用于大量生产。     

水热还原法合成LiFePO4及电化学性能研究

以可溶性三价铁盐FeCl3为铁源,Fe粉作还原剂,应用水热还原法合成LiFePO4.XRD、红外光谱及SEM形貌表征表明,在水热条件下,铁粉能完全将三价铁还原为二价铁,得到单一相LiFePO4,且其颗粒团聚形成花簇状;而LiFePO4经过葡萄糖的热解包覆碳生成LiFePO4/C后,颗粒转变似球状.电化学性能测试结果表明,虽然单相LiFePO4的放电容量很低,但LiFePO4/C却表现出良好的倍率性能和循环稳定性.     

Oxygen vacancy rich tungsten oxide with nitrogen doped mesoporous carbon as matrix for overall water splitting and 4-nitrophenol reductive removal

A nitrogen doped mesoporous carbon matrix supported oxygen vacancies rich tungsten oxide composite material, WO_3-x@NC (1 > x > 0), has been fabricated successfully with chitosan and H₃PW₁₂O₄₀ as precursors through calcination. In this composite material, WO_3-x particles with the size about 10–15 nm disperse evenly in nitrogen doped mesoporous carbon matrix. WO_3-x@NC presents low overpotentials (η₁₀) of 61 and 306 mV to reach a current density of 10 mA/cm² for HER and OER in 1.0 M KOH, respectively. With WO_3-x@NC as both cathode and anode at the same time, an electrolyzer, WO_3-x@NC//WO_3-x@NC was constructed for overall water splitting, which only needs a cell voltage of 1.60 V to achieve a current of 10 mA/cm². During this process, WO_3-x@NC//WO_3-x@NC exhibits remarkable stability in 48 h. Moreover, besides HER and OER, WO_3-x@NC also shows striking catalytic activity for reductive conversion of 4-nitrophenol to 4-aminophenol. Oxygen vacancies from WO_3-x and good electron transportation property of nitrogen doped carbon matrix play important roles in overall water electrocatalytic splitting and 4-nitrophenol reductive removal. We expect WO_3-x@NC will find its way as a new resource for hydrogen energy as well as a promising material in 4-nitrophenol removal from water.     

Synthesis of 4-aminopolymethoxycoumarins from 4-hydroxycoumarin triflates

4-Aminocoumarins were synthesized in high yields by the reaction of 4-hydroxycoumarin trifluoromethanesulfonates with amines. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1583–1588, September, 2006.     

Synthesis of 4-Aminosalicylglycine

To search for a better prodrug of 4-aminosalicylic acid that is expected to deliver stably parent drug to colon against the inflammatory bowel disease, a novel 4-aminosalicylic acid derivative was designed and synthesized from 4-aminosalicylic acid. 4-Aminosalicylglycine was prepared from 4-aminosalicylic acid by protecting amino and hydroxyl groups with benzyloxycarbonyl and acetyl, respectively, then the carboxylic acid was converted to acyl chloride which was treated with glycine. After removing the protection groups, 4-aminosalicylglycine wasobtained. All the compounds were characterized by FT-IR, ^1H-NMR, ^13C-NMR spectra. In vivo experiment on rats suggested that the curative effect of 4-aminosalicylglycine was more effective than that of 4-aminosalicylic acid.