直接桃红B(C.I.直接红9)的合成研究

三聚氯氰与H酸单钠盐一次缩合反应得到一缩合物A,一缩合物A与脱氢硫代对甲苯胺单磺酸二次缩合反应得到二缩合物B,二缩合物B与邻氨基苯甲酸的重氮盐偶合后得到偶氮物C,偶氮物C再在碱性溶液中进行水解反应得到直接桃红B(C.I.Direct Red 9)。本论文对于一次缩合、二次缩合、偶合、水解反应的反应条件进行探讨,找出了直接桃红B适宜的合成反应条件。     

一种荧光增白剂的合成与应用

为了专利号为200810016962涉及一系列含2,5-二磺酸苯胺基团季铵盐型荧光增白剂及其合成与应用。该系列增白剂采用以下合成步骤:(1)0～5℃下三聚氯氰与2,5-二磺酸苯胺反应2.5h,pH控制在1.8～2.1合成一步缩合产物;     

四磺酸基液体荧光增白剂的制备与性能

通过DSD酸钠与三聚氯氰缩合 ,再分别与氨基苯磺酸盐和乙醇胺进行缩合 ,通过控制适当的温度和pH制得四磺酸基液体荧光增白剂。重点探讨了其合成条件和应用效果     

醛基型三苯二噁嗪活性染料的合成与应用

将2,5-二氨基苯磺酸通过缩合反应连接到四氯苯醌的2,5位碳原子上,得到染料中间体Ⅰ;然后在微波条件下氧化闭环,得到中间体Ⅱ(染料母体);中间体Ⅱ与戊二醛前体的溴代物缩合、水解,得到目标产物。采用正交试验获得微波条件下氧化闭环反应的最佳工艺参数为:微波功率120W,辐射时间15min,浓硫酸用量为中间体Ⅰ的22倍,在此条件下中间体Ⅱ的产率为86%。通过质谱(ESI-MS)、红外(FT-IR)和紫外(UV-vis)对目标产物进行表征,并进行了皮革染色试验。结果表明:目标产物的各项色牢度均达到4级以上,具备了活性染料的特征。     

2,5-二甲氧基对-β-硫酸酯乙基砜苯胺的合成工艺研究

本文研究了以2,5-二甲氧基苯胺为原料,经过乙酰化、氯磺化、还原、缩合及酯化反应制得染料中间体2,5-二甲氧基对-β-硫酸酯乙基砜苯胺的合成工艺。经过实验得到最佳工艺条件是:n(2,5-二甲氧基苯胺)∶n(乙酸酐)∶n(氯磺酸)∶n(亚硫酸氢钠)∶n(环氧乙烷)∶n(硫酸)=1.00∶1.14∶10.00∶2.50∶9.00∶1.60,氯磺化反应的保温温度为30℃～32℃。     

聚酰胺改性荧光增白剂的制备及其在造纸中的应用

三聚氯氰与4,4'-二氨基二苯乙烯-2,2'-二磺酸和2种氨基化合物经过三步缩合反应可得到三嗪基氨基二苯乙烯型荧光增白剂,本文用聚己二酰二乙烯三胺(PPC)代替其中一种氨基化合物,合成聚酰胺改性高分子荧光增白剂(PPC-FBs).实验显示,在纸张涂布中使用PPC-FBs,纸张的白度以及耐光性均得到明显改善.确定了PPC-FBs在涂布颜料中的适宜用量.     

4,4'-二氨基二苯胺-2-磺酸的合成及其结构表征

本文以2-氯-5-硝基苯磺酸和对苯二胺为原料,通过缩合和还原两步反应,合成了无致癌性染料中间体4,4'-二氨基二苯胺-2-磺酸.利用红外光谱、质谱、氢核磁共振谱对合成产物进行了结构表征.     

4,4′-二氨基二苯胺-2-磺酸的合成及其结构表征

本文以 2 -氯 - 5-硝基苯磺酸和对苯二胺为原料 ,通过缩合和还原两步反应 ,合成了无致癌性染料中间体4 ,4′-二氨基二苯胺 - 2 -磺酸。利用红外光谱、质谱、氢核磁共振谱对合成产物进行了结构表征。     

树枝状大分子PAMAM-FBs合成及其在造纸中的应用

两种氨基化合物和三聚氯氰与4,4＇-二氨基二苯乙烯-2,2＇-二磺酸经过三步缩合反应可得到三嗪基氨基二苯乙烯型荧光增白剂.本文使用（PAMAM） 1.0 G,代替一种氨基化合物,合成一种高分子荧光增白剂（PAMAM-FBs）.实验显示,使用PAMAM-FBs对纸张涂布处理时最佳用量为5‰,滤纸的的白度和耐光性均得到明显改善.     

树枝状大分子PAMAM—FBs合成及其在造纸中的应用

2种氨基化合物和三聚氯氰与4,4’-二氨基二苯乙烯-2,2’-二磺酸经过三步缩合反应可得到三嗪基氨基二苯乙烯型荧光增白剂,本文使用（PAMAM）1．0G,代替一种氨基化合物,合成一种高分子荧光增白剂（PAMAM—FBs）。实验显示,使用PAMAM—FBs对纸张涂布处理,PAMAM—FBs在涂布颜料中的最佳用量为5‰,滤纸的的白度以和耐光性均得到明显改善。     

麦芽糖醇硬脂酸酯的合成研究

以麦芽糖醇、硬脂酰氯为主要原料,在催化剂存在下,在醋酸溶剂中缩合成麦芽糖醇硬脂酸酯。通过考察催化剂种类及用量、溶剂的用量、反应温度、反应时间、原料配比等对反应的影响,确定了最佳反应条件。     

New black tea polyphenol having N-ethyl-2-pyrrolidinone moiety derived from tea amino acid theanine: isolation,characterization and partial synthesis

Ethylpyrrolidinonyl theasinensin A, a novel polyphenol having a N-ethyl-2-pyrrolidinone moiety, was isolated from commercial black tea, and the structure was determined on the basis of spectroscopic analysis and chemical synthesis, which was achieved by condensation of theasinensin A with N-ethyl-5-hydroxy-2-pyrrolidinone. The N-ethyl-5-hydroxy-2-pyrrolidinone is spontaneously produced from theanine Strecker aldehyde by intramolecular cyclization; therefore, the presence of ethylpyrrolidinonyl theasinensin A in black tea suggested that theanine, the most abundant amino acid in tea leaf, was degraded to a Strecker aldehyde and conjugated with polyphenol A-rings during black tea production.     

Nucleophilic reactions of sorbic acid

The conjugated dienoic acid structure of sorbic acid renders it susceptible to nucleophilic attack. Nucleophiles known to react with sorbic acid include sulphite ion and amines. These attack the molecule in position 5 and, in the cse of amines, cyclization to form substituted dihydropyridones may follow. Recent investigations show that thiols in general can also add to sorbic acid. Cysteine, for example, reacts slowly with sorbic acid at 80 degrees C and pH 5.5, leading to 5-substituted 3-hexenoic acid. In general, reaction products are difficult to isolate from aqueous reaction mixtures as they are susceptible to acid- and base-catalysed hydrolysis. A synthesis of model compounds may be carried out by reaction of sorbate esters with the appropriate thiol (or its ester if it is an acid) in the presence of the corresponding sodium alkoxide. It is interesting that alkyl thiols give di-adducts with sorbate ester whilst low molecular weight thiols containing an oxygen atom give a monoadduct. The mechanism of this reaction and its implications to the preparation of samples for toxicological evaluation are discussed. The reaction of sorbic acid with nitrite ion is unusual and its mechanism is considered.     

扎托布洛芬的合成工艺改进

目的 改进扎托布洛芬的合成工艺.方法 以邻氯苯乙酮和苯硫酚为原料,经Ullmann缩合、Willgerodt重排、闭环、Friedel.craRs反应和1,2-芳香基重排等8步反应制得扎托布洛芬.结果 总收率9.9%.结论 本工艺操作简便,成本较低,适于工业化生产.     

A Study on the Condensation of Sorbose with Acetone: Catalysis by Macroporous Ion Exchange Resins

A study on the condensation of L-sorbose with acetone to form 2,3-4,6-di-o-isopropylidene sorbose (diacetone sorbose, DAS) in the presence of various macroporous cationic exchange resins (sulfonic acid type based on styrene and divinyl benzene copolymers) has been carried out. The condensation rates were found to be dependent on the characteristics of the resins such as surface area and percent crosslinking. The formation of DAS was found to increase with increase in temperature and decrease with increase in particle size of the sorbose. On continuous use of the resins in the reaction the catalytic activity is found to decrease.     

Effect of Browning Reactions on the Formation of Flavour Substances

Nonenzymic browning reactions are usually accompanied by side reactions resulting in the formation of various flavour substances. The amount of volatile flavour compounds is very low in comparison with that of brown pigments. Flavour compounds are formed from intermediary reaction products by several secondary reactions: 1. cyclization of oligosubstituted hydroxylic, thiol, amine, carboxylic and carbonylic derivatives; 2. condensation of volatile carbonylic derivatives with amine, sulphur, or other carbonylic derivatives; 3. Strecker degradation of amino acids and peptides by quinones, osones, and triosones; 4. aldolization of aldehydes, especially in presence of amines; 5. spontaneous or thermic decomposition of macromolecular brown pigments or intermediary Schiff bases; 6. binding of flavour compounds into flavour-neutral or modified-flavour derivatives. By modifying the composition of ingredients or by adjusting the processing and storage conditions it is possible to obtain desirable flavour properties.     

7种氨基酸与丙烯醛典型反应产物的表征

为探究油炸薯片中的内源有害物丙烯醛产生后显著消减的原因,本研究利用马铃薯中7种含量较高的氨基酸(甘氨酸、天冬酰胺、天冬氨酸、谷氨酸、谷氨酰胺、缬氨酸、苏氨酸)与丙烯醛在不同温度及时间条件下反应,对反应产物进行分离纯化和结构鉴定,研究氨基酸对丙烯醛的清除作用及其作用机理.研究发现,所选氨基酸可高效消除丙烯醛,并生成8种首...     

芳香族甜菜碱型加脂复鞣剂的合成与表征

通过对羟基苯磺酸、苯酚、单宁及甲醛的共缩合,以及缩合产物对环氧季氨盐的亲核开环反应,合成了带有C18烷烃链的芳香族甜菜型加脂复鞣剂。利用红外光谱（FT-IR）和差示扫描量热法（DSC）对中间物及产物结构进行了跟踪表征。结果表明：反应过程中官能团的变化证实了产物的合成,产物中C18烷烃链的引入导致Tm大大降低,起到了明显的内增塑作用。     

Function of second glucan binding site including tyrosines 54 and 101 in Thermus aquaticus amylomaltase

Amylomaltase from Thermus aquaticus catalyzes three types of transglycosylation reaction, as well as a weak hydrolytic reaction of alpha-1,4 glucan. From our previous study [Fujii et al., Appl. Environ. Microbiol., 71, 5823-5827 (2005)], tyrosine 54 (Y54) was identified as an amino acid controlling the reaction specificity of this enzyme. Since Y54 is not located around the active site but in the proposed second glucan binding site that is 14 A away from catalytic residues, the functions of Y54 and the second glucan binding site are of great interest. In this study, we introduced mutations into another tyrosine (Y101) in the second glucan binding site. The obtained mutated enzymes were subjected to all four types of enzyme assay and the effects of mutations on the reaction specificities of these enzymes were comprehensively investigated. These studies indicated that the amino acid substitution at Y54 or Y101 for removing their aromatic side chain increases cyclization activity (intra-molecular transglycosylation reaction) but decreases disproportionation, coupling and hydrolytic activities (inter-molecular reactions). The superimposition of the reported structures of the enzyme with and without substrate analog revealed the occurrence of a conformational change in which a donor binding site becomes open. From lines of evidence, we conclude that the binding of glucan substrate to the second glucan binding site through an interaction with the aromatic side chains of Y54 and Y101 is a trigger for the enzyme to take a completely active conformation for all four types of activity, but prevents the cyclization reaction to occur since the flexibility of the glucan is restricted by such binding.     

环（组氨酸-脯氨酸）二肽的高温高压辅助合成工艺优化

将高温高压技术应用于环（组氨酸-脯氨酸）二肽（cyclo(His-Pro),CHP）的制备。以二肽甲酯盐酸盐为原料,采用高温高压辅助环化法在水中制备CHP,通过单因素试验考察了各种反应变量如压力、时间、溶液pH值以及底物质量浓度对CHP产率的影响,采用正交试验对高温高压辅助环化工艺条件进行优化。采用超高效液相色谱法和电喷雾质谱技术对产物中的CHP进行定量和定性分析。结果表明,最佳的反应条件为：反应压力0.20 MPa、反应时间3.5 h、溶液pH 6.0、底物质量浓度15 mg/mL。在此条件下可以得到较高产率（91.35%）的CHP,并且反应中没有观察到消旋。与传统的甲醇回流法相比,本研究的环化方法省时、高效、环保,并且能够得到较高的产率,同时产物没有发生消旋。