测镉新试剂2—羧基—4—溴苯重氮氨基偶氮苯的合成及该类试剂结构与分析性能

合成了新的测镉试剂２－羧基－４－溴苯重氮氨基偶氮苯并研究了在ＴｒｉｔｏｎＸ－１００存在下与镉的显色反应。把该显色反应结果与同类试剂邻羧基苯重氮氨基偶氮苯、间羧基苯重氮氨基偶氮苯、对羧基苯重氮氨基偶氮苯、２，４－二溴－６－羧基苯重氮氨基偶氮苯和２，６－二溴－４－羧基苯重氮氨基偶氮苯与镉的显色反应进行了比较，从而讨论了试剂结构与分析性能之间的关系。     

2—苯胺—4—甲基—6—三氟甲—1,3,5—三嗪衍生物的合成及其除草活性

合成了２－苯胺１,３,５三嗪的一系列衍生物,并评价了它们的除草活性。首先研究了三嗪环上的取代,结果表明４－甲基－６－三氟甲基衍生物显示高的除草活性,其次研究了２－苯胺－４－甲基－６－三氟甲基－１,３,５－三嗪的苯环取代,结果表明苯环上的３－或４－卤素衍生物显示更高的除草活性。在盆栽试验中表现高除草活性的２－（３－氯苯胺基）－４－甲基－６－三氟甲基－１,３,５－三嗪和２－（４－氯苯胺基）－４－甲基－     

3—甲氧基—4—吗啉基苯基重氮四氯化锡复盐合成与表征

应用染料中间体红色基Ｂ为原料，经重氮化、氯代、还原和重氮成盐等步骤合成了一种重氮光敏试剂３－甲氧基－４－吗啉基苯基重氮四氯化锡复盐，并通过紫外光谱、红外光谱、核磁共振氢谱元素分析等手段对产物及两个中间产品进行了结构表征。     

4—甲基—2—环戊基苯腈和1—氰基—4—甲基—1,4—二环戊基—2,5—环己二烯的合成

本文在进行甲基苯腈与溴化环戊烷的烷基化反应同时，发现有特殊的烷基加成反应发生，得到两种新化合物４－甲基－２－环戊基苯腈和１－氰基－４－甲基－１，４－二环戊基－２，５－环己二烯，并对其结构进行了鉴定。     

DBU——一种大有可为的试剂

最近发现，ＤＢＵ（１，８－二氮杂环环（５，４，０）７－十一烯）在合成α－重氮酮和α－重氮酯的反应中有很好的催化作用，在ＤＢＵ作用下，α－溴丙二酸酯衍生物可以和Ｃ６０发生反应。     

4—氨基—3—溴—苯磺酰基乙酸及染料的合成和脱羧研究

以４－氨基－苯磺酰基乙酸为原料，用氢溴酸和双氧水溴化，合成了４－氨基－３－溴－苯磺酸基乙酸，并以此为重氮组分，合成了三支含溴偶氮染料，进行了热重脱羧研究，结果表明，染料的脱羧温度符合分散染料热熔法染色的温度要求。     

测镉新试剂2－羧基－4－溴苯重氮氨基偶氮苯的合成及该类试剂结构与分析性能关系的研究

合成了新的测镉试剂２－羧基－４－溴苯重氮氨基偶氯苯并研究了在ＴｒｉｔｏｎＸ－１００存在下与镉的显色反应。把该显色反应结果与同类试剂邻羧基苯重氮氨基偶氮苯、间羧基苯重氮氨基偶氮苯、对羧基苯重氮氨基偶氮苯、２，４－二溴－６－羧基苯重氮氨基偶氮苯和２，６－二溴－４－羧基苯重氮氨基偶氮苯与镉的显色反应进行了比较，从而讨论了试剂结构与分析性能之间的关系。     

2—甲基—3（4）—呋喃硫醇的合成

从２－甲基－３（４）－乙酰硫基呋喃合成了香料化合物２－甲基－３（４）－呋喃硫醇，并对产品进行了分析鉴定。     

4—甲氧基—2—甲基溴苯的高选择性溴代合成

本文研究了通过了３－甲基苯甲醚选择单溴代合成４－甲氧基－２－甲基溴苯的合成方法并选择了较佳合成条件。     

N—甲基—N—羟乙基苯胺制备

以Ｎ－甲基苯胺和环氧乙烷为原料，采用气相非均相法合成了Ｎ－甲基－Ｎ－羟乙基苯胺。在反应温度１２０－１４０℃，反应压力０．４－０．６ＭＰａ，催化剂 ０．３％－０．４％的条件下，得到了较好的产品质量和收率。     

抗肿瘤药替莫唑胺的合成

以5-氨基-3H-咪唑-4-甲酰胺盐酸盐为原料,经重氮化反应合成5-重氮基-3H-咪唑-4-甲酰胺,然后在极性溶液和催化剂存在下与甲基异氰酸酯反应合成替莫唑胺,后者反应时间短,为20h,收率达76.5%。     

Synthesis and application of yellow azo‐anthraquinone disperse dyes for polylactide fibres

1‐Phenyl‐3‐methyl‐5‐pyrazolonyl azo‐anthraquinone dyes having high light fastness on polylactide fibres were synthesised from 1‐aminoanthraquinone via a diazotisation‐coupling reaction with 1‐phenyl‐3‐methyl‐5‐pyrazolones. The structures of these new dyes were confirmed using mass spectrometry, infrared and proton nuclear magnetic resonance spectroscopy and combustion analyses. Their dyeing behaviour on polylactide fibres was also determined, whereupon it was found that the title dyes could be applied at a relatively low dyeing temperature and that the corresponding dyed fabrics had good fastness properties.     

Synthesis and absorption spectra of some novel hetaryldisazocalix[4]arene derivatives

In this study, a convenient method for the synthesis of thirteen novel disazo dyes containing 25,26,27‐tribenzoyloxy‐28‐hydroxycalix[4]arene have been described. 5,11,17,23‐Tetra‐tert‐butyl‐25,26,27,28‐tetrahydroxycalix[4]arene, 25,26,27,28‐tetrahydroxycalix[4]arene and 25,26,27‐tribenzoyloxy‐28‐hydroxycalix[4]arene were synthesised based on previously published literature. 2‐Arylhdrazone‐3‐ketiminobutyronitriles were synthesised and reacted with hydrazine hydrate to afford the corresponding 5‐amino‐4‐arylazo‐3‐methyl‐1H‐pyrazoles. Thirteen novel hetaryldisazocalix[4]arene derivatives were achieved by diazotisation of 5‐amino‐4‐arylazo‐3‐methyl‐1H‐pyrazoles using nitrosylsulphuric acid, coupled with 25,26,27‐tribenzoyloxy‐28‐hydroxycalix[4]arene. The obtained hetaryldisazocalix[4]arene dyes were characterised based on Fourier Transform–infrared, proton nuclear magnetic resonance and mass spectroscopic techniques, as well as elemental analysis. The solvatochromic behaviour of these dyes in various solvents was examined. Acid‐base effects on the visible absorption maxima of the dyes were also reported.     

Solubilisation kinetics of some monoazo naphthalimide disperse dyes containing butyric acid and investigation of fastness properties of the dyes on polyester

In this paper, the solubilisation kinetics of three novel monoazo disperse dyes based on naphthalimdes incorporating a butyric acid group were investigated in different conditions using spectrophotometry. All dyes showed a reasonable level of solubilisation in alkaline media. Kinetic studies of the solubilisation reaction of the dyes in alkaline media showed that the rate of solubilisation of all dyes is a pseudo first‐order reaction equation. The rate constants of the solubilisation reaction of the dyes in alkaline media indicated that dye 3 , which is prepared by the diazotisation of 4‐amino‐n‐butyric acid 1,8‐naphthalimide and coupled with N,N‐diethy‐n‐hydroxyethyllaniline, has the highest rate of reaction and dye 1 , which is prepared by the diazotisation of 4‐amino‐n‐butyric acid 1,8‐naphthalimide and coupled with N,N‐diethylaniline, has the lowest rate. The dyes were applied on polyester fabrics and their fastness properties were examined. The dyed fabrics showed a good to excellent degree of wash and rubbing fastnesses after replacing reduction clearing with alkali clearing.     

(S)-(+)-γ-苄氧基甲基-γ-丁内酯的合成研究

以Ｌ 谷氨酸为原料,首先在－５～０℃条件下重氮化,随后常温内酯化,然后在对甲苯磺酸催化下于苯中回流进行酯化,用硼氢化钠在常温下还原,最后用氧化银作为碱发生常温威廉逊（Ｗｉｌｉａｍｓｏｎ）醚化反应,以３２３％的总产率合成了标题化合物。     

Substituent effects on the colour,dyeing and fastness properties of 4-phenylazo-1-naphthylamines and of 2-acetylamino-5-methoxy-4-N-ß-cyanoethyl-N-ß-hydroxyethylaminoazobenzene

The synthesis of a series of blue disperse dyes obtained by diazotisation of substituted anilines and coupling with 2-acetylamino-5-methoxy-4-N-ß-cyanoethyl-N-ß-hydroxyethylaniline and to N-ß-hydroxyethyl-1-naphthylamine is described. Substituent effects on the colour of the dyes is discussed, with particular respect to analogous dyes derived from 4-N-ß-cyanoethyl-N-ß-hydroxythylaniline. Some dyes from trisubstituted anilines as diazo component colour polyester in deep blue shades of generally good fastness properties.     

混合偶合法一步合成活性黑染料

将对位酯重氮化，与J酸—三聚氯氰缩合物(0．003mol)、H酸—对位酯偶氮化合物(0．009mol)在同一个反应体系中用混合偶合法同时合成了C．I．活性黑5和一只橙色活性染料，改变偶合组分比例和反应条件，可得到色光不同的黑色活性染料。控制合成过程中产生的杂色染料，可以控制染料产品的色光和应用性能。     

Synthesis of some new azopyrazole dyes

A variety of new azopyrazolo [1,5-c]-as-triazine dyes have been synthesised via diazotisation of 3-amino-4-arylazo-1-pyrazolin-5-one and coupling with active hydrogen reagents. These dyed nylon 6, nylon 66, acrylic, polyester, silk and wool with colours ranging from scarlet red to dark brown and may find useful applications.     

4-(2''''-甲氧基乙基)苯酚的制备

本文以对硝基甲苯和多聚甲醛为原料,经缩合、甲基化、还原、重氮化、水解等反应制备了合成美多心安的重要中间体4-(2′-甲氧基乙基)苯酚, 并对该路线的关健步骤——对硝基甲苯与多聚甲醛的缩合反应条件进行了优化,得出了较合理的条件为: 溶剂：DMSO; 催化剂:苯酚钾; 配料比：2.50-1.67。 该条件下对硝基甲苯的转化率及选择率可达31%和72%。未反应的对硝基甲苯可回收套用。     

Synthesis of disazo dyes derived from heterocyclic components

In this study, 2-phenylhydrazone-3-ketiminobutyronitrile was synthesised and reacted with hydrazine hydrate and phenylhydrazine to afford the corresponding 5-amino-3-methyl-4-phenylazo-1H-pyrazole and 5-amino-3-methyl-4-phenylazo-1-phenylpyrazole, respectively. Ten novel disazo dyes were then synthesised by diazotisation of 5-amino-3-methyl-4-phenylazo-1H-pyrazole and 5-amino-3-methyl-4-phenylazo-1-phenylpyrazole using nitrosylsulphuric acid, and coupling with 4-hydroxy-6-methyl-2-pyrone, 4-hydroxycoumarin, 3-methyl-1H-pyrazolin-5-one, 3-methyl-1-phenylpyrazolin-5-one and 3-cyano-6-hydroxy-4-methyl-2-pyridone. The dyes were characterised by elemental analysis and spectral methods. The solvatochromic behaviour of these disazo dyes in various solvents was evaluated. Received: 18 May 2005; Accepted: 8 July 2005.