3-(4-氨基苯基偶氮)苯磺酸钠的合成

氨基甲基苯基偶氮苯磺酸钠;3-(4-氨基苯基偶氮)苯磺酸钠的合成     

邻异丙基苯酚的合成及其与对氨基苯磺酸的偶合

苯酚和异丙醇在有ＢＦ３－乙醚存在的磷酸溶液中反应，得６０％左右收率的邻异丙基苯酚，产物与对氨基苯磺酸偶合得化合物２－（４－磺酸基苯偶氮）－６－异丙基苯酚。合成涉及Ｆｒｉｅｄｅｌ－Ｃｒａｆｔｓ、重氮化、偶合等重要反应以及许多有机实验操作。     

4—（4—氨基—3—甲基苯偶氮）苯磺酸的合成

４－（４－氨基－３－甲基苯偶氮）苯磺酸可做为染料中间体［１］．据其结构，一般认为可由对氨基苯磺酸重氮盐与邻甲苯胺通过偶合反应制备．初步实验表明，对氨基苯磺酸重氮盐与邻甲苯胺在弱酸及弱碱性介质下易发生氨基上的偶合反应，生成重氮氨基化合物；在强酸性介质下...     

对-偶氮苯重氮氨基偶氮苯磺酸与钯的显色反应研究及其应用

本文研究了对-偶氮苯重氮氨基偶氮苯磺酸在非离子表面活性剂Tween-80存在下,与钯(Ⅱ)显色反应适宜条件.实验结果表明,在pH10.80～11.10范围内钯(Ⅱ)与题示试剂形成1:4的橙红色络合物,其最大吸收峰位于533nm处,试剂最大吸收为440nm,其对比度达93nm.钯(Ⅱ)在0～30μg/25ml范围内遵守比耳定律,并由此计算出其表观摩尔吸光系数ε_(533)=1.0×10~5L.mol~(-1).cm~(-1)。该方法用于催化剂中微量钯的测定,获得了令人满意的结果。     

染料中间体间氨基-N-取代-苯磺酰胺的合成研究

以间氨基苯磺酸为原料，经乙酰化保护氨基，用氯磺酸／氯化亚砜将磺箕转变为磺酰氯，再分别与氨基G酸、吐氏酸、γ－酸、6－氨基－1，3－萘二磺酸、5，6－二氨基－1，3－萘二磺酸胺化缩合，水解去乙酰基，较高收率地合成了间氨基－N－取代－苯磺酰胺类染料中间体。产物结构经元素分析、红外、核磁和质谱确证。     

3-氨基-4-氨甲基苯磺酸钠的合成与表征

以邻硝基甲苯为原料,经磺化,光氯化,Holfmann氨化及水合肼还原合成了未见文献报道的3-氨基4-氨甲基苯磺酸钠,其结构经^1H NMR,IR,MS及元素分析表征。纯度达99．2％（HPLC）,总收率62．8％。     

一类芳香族偶氮化合物的合成及表征

采用重氮偶合反应合成了一系列不同对位取代的4-[N，N-(二羟乙基)]氨基偶氮苯化合物，其结构用元素分析，IR，1HNMR，DSC，DSC等进行表征和确认。     

新显色剂N—烯丙基—N^1—（氨基对苯磺酸钠）硫脲与铜（Ⅱ）显色反应的研…

本研究了新合成的显色剂Ｎ－烯丙基Ｎ＇－（氨基对苯磺酸钠）硫脲与铜（Ⅱ）发生显色反应的条件实验，结果发现，在ｐＨ３．６－５．４的ＨＡｃ－ＮａＡｃ体系中，铜和显色剂形成１：３的蓝色水溶性络合物，最大吸收波长为３０３ｎｍ，摩尔吸光系数为１．３４×１０＾５Ｌ·ｍｏｌ＾－１·ｃｍ＾－１Ｃｕ（Ⅱ）在５－４０μｇ／２５ｍｌ遵从比尔定律，相关系数ｒ＝０．９９９６，将此方法应用于铝矿样，头发和麦麸中微量铜的测定，     

对氨基苯磺酸钠的光化学动力学的ESR研究

The photochemical degradation kinetics of Sodium pamino-Phenyl Sulphonate in aqueous solution and CdS colloid systems was studied by means of ESR method, and the kinetics behaviour for both the photoreactions in aqueous solution system and in CdS colloid system was compared. The results indicated that both the initial concentrations of SSN and the presence of CdS colloid obviously affected the photodegradation processes of SSN in the way of enhancing the rate constants for the formation of free radical SO3-•. The kinetics processes of photoreartions were treated by the quasi-stationary analysis method, the results of analysis are consistent with the phenomena observed in our experiments. The experimental results were briefly analyzed and discussed.     

偶氮基杯芳烃化合物的合成及其偶氮-醌腙互变异构性质

通过芳胺的重氮化-偶合反应合成了8个偶氮基杯芳烃化合物, 其结构经IR, 1H NMR, ESI-MS和元素分析表征. 通过UV-Vis, 1H NMR和IR考察了溶液pH值对所合成化合物5,11,17,23-四[(2-苯并噻唑基)偶氮基]-25,26,27,28-四羟基杯芳烃(3)和5,17-二[(1-萘基)偶氮基]-25,26,27,28-四羟基杯芳烃(4)的偶氮-醌腙互变异构的影响. 结果表明, 随着溶液pH值增加, 醌腙体在偶氮-醌腙互变异构平衡中的比例增加, 当pH≥10时, 几乎全部转变为醌腙体. 特别当溶液pH=-1时, 化合物4可以形成一种大的共轭体系, 使其λmax由477 nm红移至545 nm.     

硫酸氢钠催化合成富马酸二乙酯的研究

以富马酸和乙醇为原料,硫酸氢钠作催化剂合成富马酸二乙酯。用正交实验讨论了最佳合成条件:反应温度130℃,n(乙醇)∶n(富马酸)=4∶1,时间6h,催化剂用量为富马酸质量的5.0%,酯化率达93.5%。该法操作简单,酯化率较高,催化剂可回收利用。     

金属钠与盐酸反应的实验研究

目前关于金属钠与盐酸或水反应速率的快慢问题,不同学者提出了不同的观点。基于此,开展了“钠与盐酸反应”的实验研究,实验中观察到白色沉淀,定性分析了白色沉淀的成分并提供了理论依据。     

Synthesis of the first tris(crown formazan)

A synthesis of tris(crown formazan) 2 from the corresponding hexakis(acetamidophenoxymethyl)benzene 11 by hydrolysis with an ethanolic solution containing hydrochloric acid followed by diazotization and subsequent coupling with cyanoacetic acid in pyridine containing CuSO₄ is described.     

Efficient Synthesis of Beraprost Sodium

An efficient and straightforward synthesis of beraprost sodium was developed with dicyclopentadiene as a starting material, a one-pot reaction product 5 as key intermediate and the Prins reaction and the Horner-Wads- worth-Emmons reaction as key steps. The structures of the key intermediate and the target compound were confirmed by ¹H NMR, ¹³C NMR and MS. The purity of beraprost sodium identified by high performance liquid chromatography(HPLC) was identical to that of Japanese Pharmacopoeia(16^th). This development will be used for the industrial synthesis of beraprost sodium.     

对氰基苯甲酸乙酯的合成研究

以对氨基苯甲酸乙酯为原料，经重氮化反应及Sandmeyer的氰化反应制得对氰基苯甲酸乙酯，对重氮盐的制备及氰化过程进行了研究，简化了操作，提高了产物收率。     

A New One-dimensional Sodium Polymer Constructed from 4-Carboxy-benzenesulfonic Acid

A new one-dimensional double chain coordination polymer, [Na(cbsH)(H2O)3]n (cbsH = 4-carboxy-benzenesulfonic anion), has been synthesized by aqueous reaction, structurally described, and thermally characterized. It crystallizes in the triclinic system, space group P with a = 5.645(4), b = 7.905(5), c = 13.043(8) , α = 89.391(7), β = 80.637(7), γ = 82.845(7)°, V = 569.8(6) 3, Z = 2, C7H11NaO8S, Mr = 278.21, Dc = 1.622 Kg/m3, F(000) = 288, R = 0.0260 and wR = 0.0697. The title compound consists of one-dimensional double chains. 4-Carboxy-benzenesulfonic acid acts as a bridging bidentate ligand to link two sodium(I) ions to form a binuclear structure. Remarkably, the sodium(I) ion behaves as a metal bridge so that the binuclear structure units are connected to construct a one-dimensional double chain polymer. Furthermore, a 3-D framework is assembled through intermolecular hydrogen bonds. Thermogravimetric analysis shows that this compound begins losing the free solvent molecules at 106 ℃ and decompounding completely at 580 ℃.     

邻羧基苯甲酰二茂铁钠的合成、晶体结构及电化学性质

参照文献方法合成了邻羧基苯甲酰二茂铁钠,首次培养得到了它的单晶．发现在其固态结构中,邻羧基苯甲酰二茂铁阴离子与四水合钠阳离子通过分子内氢键相互作用;分子间的氢键又把多个二茂铁衍生物分子连接成二维的网状结构．研究了标题化合物在甲醇溶液中的电化学性质．     

Synthesis of 1‐(p‐Sulphophenyl)‐3‐methyl‐5‐pyrazolone Based Acid Dyes and Their Applications on Leather

A new series of pyrazolone based azo acid dyes (3a–g) has been synthesized starting from 1‐(p‐sul‐phophenyl)‐3‐methyl‐5‐pyrazolone (1). The synthetic methodology included the nitrosation of p‐sulphophenyl methyl pyrazolone followed by reduction, diazotization and coupling with Naphthol AS derivatives (2a–f), in alkaline medium to yield different acid dyes. Multichromic metal complexes of these dyes (5a–f, 6a–f and 7a–f) with 3d transition metals Chromium, Iron and Copper were also synthesized. The structures of all of newly synthesized compounds were confirmed by analytical data and spectroscopic techniques. The synthesized dyes were applied on leather to assess their light fastness, wash fastness and rubbing fastness and were shown to exhibit high values of 4–5 for majority of dyes.     

5-(取代吡唑基-4-次甲基)(硫代)巴比妥酸的合成

以冰乙酸为催化剂,将取代吡唑甲醛和巴比妥酸或硫代巴比妥酸在无水乙醇中进行Knoevenagel缩合反应,合成了6个5-（取代吡唑基-4-次甲基）（硫代）巴比妥酸。标题化合物经IR、1^HNMR、元素分析确证结构。     

Synthesis,Structure, Photoluminescence and Thermal Properties of Sodium Ethene‐Bis‐Nitrobenzenesulfonate

Abstract. Sodium ethene‐bis‐nitrobenzenesulfonate, [Na₂(ENS) · 6H₂O]_n( 1 ) was synthesized through coupling reaction of o‐nitrotoluenesulfonic acid in NaOH solution and characterized by single crystal X‐ray diffraction, elemental analysis, IR and ¹H NMR spectroscopy, XRPD, DSC and TGA (where ENS^2– = ethene‐bis‐nitrobenzenesulfonate). The asymmetrical unit of ( 1 ) consists of two octahedral Na^I ions, and the neighboring metal centers are bridged by μ₂ water molecules resulting in the formation of an inorganic tetranuclear unit. The tetranuclear units were connected through the ENS^2– ligands into a 2D topology net. The weak π–π stacking and H‐bonding interactions further stabilized the structure. The crystals of (C₇H₆NO₅S)^– · (H₅O₂)⁺ ( 2 ) were obtained by post‐processing the unreacted raw material to recycle. Furthermore, the rigidity and the conjugation effect of the aromatic system in compound 1 were increased through the coordination interactions of metal atoms to ligands, resulting in the emission coming from ligand enhanced with red‐shifting about 9 nm of the maximal wavelength. The conjugation effects and the steric arrangement of the substituent groups play the main role to the luminescence intensity and red‐shift effect.