(2-羟基-3-丁氧基)丙基-羧甲基壳聚糖的合成及表面性质

(2-羟基-3-丁氧基)丙基-羧甲基壳聚糖的合成及表面性质;壳聚糖衍生物; (羟基丁氧基)丙基-羧甲基壳聚糖;表面活性;表面压     

2-羟基-3-三乙氨基丙基辛基硫醚(HAPOS)对Au(Ⅲ)的萃取作用

研究了新型表面活性剂 2 羟基 3 三乙氨基丙基辛基硫醚 (HAPOS) ,在酸性条件下对Au(Ⅲ )的萃取分离作用。在实验条件下 ,一次萃取率可达 95%以上 ,并具有较高的选择性。     

3-三氟-2-羟基/氨基-1-氟代丙基膦酸酯的合成

Reaction of diethyl 2,2-difluoro-3-（a-methylbenzyl）imino-4,4,4-trifluoropropanephosphonate （3） with triethylamine afforded a mixture of normal [1,3]-proton shift reaction product 5 and its HF-eliminated compound 6Z in 1 ： 1 ratio. Upon hydrolysis, this reaction mixture gave solely 1,3,3,3-tetrafluoro-2-dioxypropanephosphonate （9）. Reaction of 3 with DBU provided only 6, in which the ratio of E/Z forms was dependent on the reaction conditions. Aqueous hydrolysis of 6 led to 9. Catalytic hydrogenation and hydrogenolysis of 6 gave geometric isomers of 11 as expected. The reaction mechanism involved was discussed.     

3-氯-2-羟基丙磺酸钠的合成工艺研究

以环氧氯丙烷（1）和NaHSO₃为原料,Na₂SO₃为引发剂,乙二胺四乙酸二钠（EDTA₂Na）为络合增效剂,经酸催化开环反应合成了磺酸型两性表面活性剂中间体--3-氯-2-羟基丙磺酸钠（2）,其结构经¹H NMR, IR和ESI-MS确证。在最佳反应条件［1 0.55 mol, n(NaHSO₃）: n（Na₂SO₃）: n（EDTA₂Na）: n（H₂O)=1.00 : 0.04 : 0.01 : 9.50, 1的滴加时间15 min,在适宜的转速（前期100 rpm, 后期300 rpm）下,于70 ℃(浴温)反应1.25 h］下合成的2,收率81.55%。并对反应机理进行了推测。     

(2-羟基-3-丁氧基)丙基-羟丙基壳聚糖的应用性质

表面活性;泡沫性;乳化性;吸湿保湿性;(2-羟基-3-丁氧基)丙基-羟丙基壳聚糖的应用性质     

2-羟基-3-(三乙胺基)丙基正癸基硫醚修饰碳糊电极测定痕量金

制备了2＿羟基＿3＿(三乙胺基)丙基正癸基硫醚修饰碳糊电极,用于痕量金的测定。研究了电极的伏安特性及分析条件。在0.2mo／LKCl-HCl缓冲溶液中(pH1),Au(Ⅲ)被富集到电极表面,然后介质交换到0.2mol／LKCl-HCl空白溶液中(pH1)进行阳极溶出伏安测定,对于5min富集,Au(Ⅲ)浓度在2×10-8～1×10-6mol／L范围内呈线性关系,检出限为1×10-8mol／L,相对标准偏差5.2%,一般常见离子不干扰。     

2-硝基-4-氯-2'-羟基-3'-特丁基- 5'-甲基偶氮苯的固相合成

2-硝基-4-氯-2'-羟基-3'-特丁基- 5'-甲基偶氮苯的固相合成;硝基氯羟基特丁基甲基偶氮苯;固相合成;重氮偶合     

2-羟基-3-(三乙胺基)丙基十烷基硫醚修饰电极测定痕量金

研究了 2 羟基 3 (三乙胺基 )丙基十烷基硫醚 (HTPSD)修饰玻碳电极测定金的伏安特性及分析条件。在 0 .2mol·L- 1KCl HCl缓冲溶液中 (pH 1) ,金 (Ⅲ )被富集到电极表面 ,然后介质交换到 0 .2mol·L- 1KCl HCl空白溶液中 (pH 1)进行阴极溶出伏安测定 ,金 (Ⅲ )浓度在 2× 10 - 81× 10 - 6mol·L- 1范围内呈线性关系。检出限为 1× 10 - 8mol·L- 1。相对标准偏差小于 6 2 % ,一般常见离子不干扰。     

2-氯-3-乙基吡啶的合成工艺研究

2-氯-3-乙基吡啶是一种重要的医药中间体,本文对其合成工艺进行研究与优化,并设计了一种新的合成方法。目标产物以2-氯烟醛为原料,经Witting反应和还原反应制得,其结构经~1H-NMR、~(13)C-NMR证实,总收率为61.6%。该方法原料廉价易得,操作简单,路线较短且收率和纯度均较高,易于实现工业化生产。     

光解苯半醌和2-羟基-2-丙基自由基的CIDEP谱

用高时间分辨ＥＳＲ波谱仪测量了光解苯半醌和２－羟基－２－丙基自由基的ＣＩＤＥＰ谱,苯半醌自由基的ＣＩＤＥＰ属ＴＭ机理,实验研究了微波功率,溶液浓度对苯半醌自由基的ＣＩＤＥＰ谱时间演化的影响,２－羟基－２－丙基自由基的ＣＩＤＥＰ属ＲＰＭ机理,实验研究了自旋极化的生成环境。     

Novel Dispersion of MWCNTs in Polystyrene Polymer Induced by the Addition of 3-Hydroxy-2-Napthoic Acid

This article reports an extensive investigation of the unique dispersion behavior of solutions with multi-walled carbon nanotubes (MWCNTs) and 3-hydroxy-2-napthoic acid (β-HNA) in tetrahydrofuran (THF) solvent, which results into a multifold enhancement in the electrical properties of polystyrene (PS). A number of solutions with 0.4% of MWCNTs (w/v) and β-HNA (0–1%, w/v) in THF were prepared separately. MWCNTs precipitated out in THF solvent shortly after the preparation and formed two distinct phase regions (2φ). Gratifyingly, addition of β-HNA solution to the MWCNTs solution offered an unprecedented enhancement in the dispersion of MWCNTs. Such dispersion in solutions with only 0.02% β-HNA (w/v) was found to be stable up to 2 weeks at room temperature. FTIR spectroscopy was incorporated to illustrate the adsorption of β-HNA onto the surface of carbon nanotubes (CNTs). After this successful dispersion, nanocomposites solutions comprising of 0.067% β-HNA (w/v), 6.7% PS (w/v), and varying concentrations of MWCNTs (0–0.33%, w/v) were prepared. A remarkable dispersion behavior of MWCNTs in the presence of polymer was also observed. Finally, thin films made up of consistent polystyrene/β-HNA concentrations and increasing amounts of MWCNTs were prepared by casting technique to investigate the influence of dispersion on the electrical properties of the film. The dispersion significantly affected the DC electrical conductivity and incorporation of 5% MWCNTs elevated the electrical conductivity up to 10 orders of magnitude with respect to neat PS.     

A Convenient Large Scale Synthesis of 2-Hydroxy-3-pinanone

A convenient large scale synthesis of 2-hydroxy-3-pinanone from readily available α-pinene has been developed. This two step method involves the diastereoselective dihydroxylation of α-pinene and subsequent oxidation of pinanediol to the hydroxyketone. The key advantages of this method, which allows access to large quantities of this important chiral auxiliary, are high yield and ease of operation.     

Triphenylphosphine-Mediated Serendipitous Synthesis of Alkyl Cinnamates Through the Reaction of 3-Hydroxy-4-Methoxybenzaldehyde and Dialkyl Acetylenedicarboxylates

Abstract

Alkyl cinnamates are formed in fairly good yields from the reaction of dialkyl acetylenedicarboxylates and 3-hydroxy-4-methoxybenzaldehyde in the presence of triphenylphosphine.     

Synthesis of 3-Hydroxy-6-Methyl- and 3-Hydroxy-2-(2-phenylethyl)pyridines and Their Sulfur-Containing Amino and Hydroxymethyl Derivatives

The aminomethylation of 3-hydroxy-6-methyl- and 3-hydroxy-2-(2-phenylethyl)pyridines by secondary amines has been investigated. It was shown that like 2-alkyl-3-hydroxypyridine aminomethylation is directed primarily to position 6 and then 4 of the pyridine ring. On heating the aminomethyl derivatives of 3-hydroxy-6-methyl- and 3-hydroxy-2-(2-phenylethyl)pyridines with acetic anhydride the corresponding acetoxy derivatives were obtained, which were converted on heating with hydrochloric or hydrobromic acids into hydroxy and bromomethyl derivatives. Isothioureidomethyl and benzimidazolylthiomethyl derivatives were synthesized by heating the bromomethyl-substituted derivative with thiourea or with 2-mercaptobenzimidazole. The structures of compounds were confirmed by data of ¹H NMR spectra. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 8, pp. 1189–1194, August, 2005.     

3-(4-羟基-2-酮基喹啉)吡唑啉的合成及其荧光性质研究

3-a,β-不饱和酮取代-4-羟基喹啉-2-酮与苯肼反应,直接成环得到一系列新型1,3,5-莞取代吡唑啉.液相和固相荧光测试结果表明该类产物是一类具有较大Stokes位移的小分子有机光学材料.吡唑啉3,5位上的取代基性质对其液相和固态荧光发射波长与发射强度有不同的影响.     

含胺基功能性单体的聚合研究——Ⅺ.甲基丙烯酸-2-羟基-3-吗啉基丙酯的合成及其聚合

<正> 一些含有吗啉基的高聚物,作为含脂肪叔胺基的医用高分子材料而被瞩目。我们曾报道了N-(N′-次甲基吗啉)取代丙烯酰胺的合成,及其在过氧化二月桂酰引发下的聚合动力学。它的聚合规律和我们以往所报道的含脂肪叔胺基单体的聚合一样。本文合成了在同—分子中既含吗啉基,又含有羟基的丙烯酸脂,即甲基丙烯酸-2-羟基-3-吗啉基丙酯(HMPMA),研究了在过氧化二月桂酰(LPO)引发下的热聚合,以及在芳香酮作增感剂下的光聚合。关于HMPMA的合成,虽有所报道,但关于其表征,在过氧化     

Synthesis and in vitro Anti-hepatitis B Virus Activity of Some Ethyl 5-Hydroxy-4-substituted Aminomethyl-2-sulfinylmethyl-1H-indole-3-carboxylates

A novel series of ethyl 5-hydroxy-4-substituted aminomethyl-2-sulfinylmethyl-1H-indole-3-carboxylates 8a―8j and 11e―11f was synthesized and evaluated in HepG2.2.15 cells for their anti-hepatitits B virus(HBV) acti-vity and cytotoxicity.Among them,six compounds showed more potent inhibitory activity than lamivudine.Compound 8e exhibited the most significant anti-HBV activity with an IC50 value of 1.62 μmol/L,which was 33-times more potent than the reference drug lamivudine(IC50=54.78 μmol/L).     

1-(2-羟基-3,5-二硝基苯基)-3-[4-(苯基偶氮)苯基]-三氮烯-阴离子表面活性剂-季铵盐型阳离子表面活性剂显色反应及其应用

在三乙醇胺介质中,新试剂1-(2-羟基-3,5-二硝基苯基)-3-[4-(苯基偶氮)苯基]-三氮烯(HDNPAPT)与季铵盐型阳离子表面活性剂及阴离子表面活性剂(AS)反应显色,形成三元络合物.研究了显色体系的条件实验,建立了测定阴离子表面活性剂十二烷基苯磺酸钠(DBOSO_3Na)、十二烷基磺酸钠(DOSO_3Na)和十二烷基硫酸钠(DSO_4Na)的方法,表观摩尔吸光系数均达10~4以上.方法已应用于环境水样中阴离子表面活性剂的测定.     

1—（2—羟基—3,5—二硝基苯基）—3—［4—（苯基偶氮）苯基］—三氮烯与汞的显色反

研究了1-（2-羟基-3,5-二硝基苯基）-3-[4（苯基偶氮）苯基]-三氮烯（HDNPAPT）试剂与汞离子的显色反应。在非离子表面活性剂TritonX-100存在下,pH10．3的NH3·H2O-NH4Cl介质中,汞与HDNPAPF形成1：4的红色络合物,表观摩尔吸光系数ε525＝1．63×105·mol-1·cm－1,汞离子浓度在0～0．64mg/L范围内符合比尔定律。方法应用于废水中微量汞的测定。     

邻香草醛荧光酮对铝的显色反应研究

研究了邻香草醛荧光酮与铝的显色反应,在表面活性剂CTMAB存在下,在pH 6.30的乙酸氨缓冲溶液介质中,铝与该试剂形成稳定络合物。其最大吸收波长位于559 nm处,表观摩尔吸光系数1.29×105L.mo-l1.cm-1,铝量在0~0.32μg/mL范围内符合比尔定律。用于石英砂样品中的铝的测定,结果满意。