微波常压法合成水杨酸酯

在浓硫酸催化下，采用微波常压法由水杨酸分别与正丁醇、异丁醇、正戊醇和异戊醇反应合成相应的水杨酸酯。结果表明：当水杨酸：醇：Ｈ２ＳＯ４＝１：５．５：０．３（摩尔比）时，采用５６０Ｗ微波辐射２２ｍｉｎ，水杨酸酯的产率可达８８．７％￣９６．４％，反应速度至少是常规反应的１４倍。     

Synthesis and Anti-inflammatory Action of （η-C5H5 ）2Ti（ Sal）2 and （η-C5H5 ）2Ti（Clo）2

IntroductionSince K pf[1]discovered that dicyclopenta die-nyltitanium dichloride possesses antitumour action in1979,a large number of cyclopentadienyltitanium com-plexes with different substituents have been synthe-sized[2,3].The experimental data reveal …     

Direct and simultaneous spectrofluorometric determination of naproxen and salicylate in human serum assisted by chemometric analysis

A direct method for the simultaneous determination of naproxen and salicylate in human serum is reported, based on a combination of spectrofluorometric measurements with two multivariate calibration techniques: partial least-squares (PLS-1) and the novel net analyte preprocessing (NAP). The method is rapid, selective and sensitive, and is based on the measurement of the fluorescence spectra of NH₃ alkalinized whole human sera at the excitation wavelength of 315 nm. It can be applied within the ranges of concentrations 50-200 ng ml⁻¹ for naproxen and 100-300 ng ml⁻¹ for salicylate. The employed chemometric techniques have been compared on the basis of the statistical indicators for calibration and validation. Reproducibility and interference studies in abnormal sera have also been carried out.     

Organogold(III) metallacyclic chemistry. Part 4. Synthesis, characterisation, and biological activity of gold(III)-thiosalicylate and -salicylate complexes

The silver(I) oxide mediated reactions of the gold(III) dichloride complex [{C₆H₃(CH₂

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uCl₂] 2a with thiosalicylic or salicylic acid gives the respective complexes [{C₆H₃(CH₂

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)-2}] 3a (X=S) or 6b (X=O), containing chelating thiosalicylate or salicylate dianion ligands. X-ray studies show that for the thiosalicylate system, the thiosalicylate sulfur atom is trans to the N,N-dimethylamino group, whereas in the structure of the salicylate complex, it is the carboxylate group that is trans to NMe₂. Both complexes show puckered metallacycles in the solid state. Electrospray mass spectrometry (ESMS) shows strong [M+H]⁺ and [2M+H]⁺ ions for both the gold-thiosalicylate and -salicylate complexes, and these ions possess a high stability towards cone voltage-induced fragmentation. ESMS was also used to identify a minor impurity, the bis(cyclo-aurated) cationic complex [A

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Me₂)-2-(OMe)-5}2]⁺ in the starting dihalide complex 2a and in the product 3a. This complex can be formed by reaction of Me₄N[AuCl₄] with 2 equivalents of the organomercury precursor [Hg{C₆H₃(CH₂NMe₂)-2-(OMe)-5}Cl]. The biological (antitumour, antimicrobial and antiviral) activities are also reported, and these reveal the complexes have moderate to high anti-tumour, antibacterial and antifungal activity.     

Synthesis and Anti-inflammatory Action of(η-C5H5)2Ti(Sal)2 and (η-C5H5)2Ti(Clo)2

Two new complexes (Cp)2Ti(Sal)2 and(Cp)2Ti(Clo)2(Cp=Cyclopentadienyl η5-C5H5), have been synthesized in anhydrous THF by the reaction of Hsal(o-hydroxybenzoic acid, salicylate acid) or Hclo[N-(m-chloro-phe-nyl) anthranili acid, acidum clofenamicum] with (Cp)2TiCl2 and characterized by means of elemental analyses, IR, 1H NMR, 13C NMR, UV and molar conductivity. In complex (Cp)2Ti(Sal)2 or (Cp)2Ti(Clo)2, the oxygen atom of the carboxyl group coordinates to Ti(IV) in a monodentate manner. The inhibitory action of the complexes on mouse ear tumefaction caused by croton oil and rat foot granulation growth caused by cotton balls is higher than that of the corresponding ligands Hsal, Hclo and [(Cp)2TiCl2], whereas their toxicity is lower than those of the free ligands.     

Synthesis,structure, spectral and magnetic properties of 4-methoxy- and 3-methylsalicylatocopper(II) complexes with 2-pyridylmethanol

The synthesis and characterization of [Cu(4-MeOsal)₂(2-pyme)₂] (1) and [Cu(3-Mesal)₂(2-pyme)₂] (2) (where 4-MeOsal?=?4-methoxysalicylate, 3-Mesal?=?3-methylsalicylate and 2-pyme?=?2-pyridylmethanol) are reported. The composition and stereochemistry as well as the mode of coordination have been determined by elemental analysis, IR, electronic and EPR spectra as well as magnetization measurements over the temperature range 1.8–300?K. The crystal structures of Cu(4-MeOsal)₂(2-pyme)₂ and Cu(3-Mesal)₂(2-pyme)₂ have been determined.     

Application of the Salicylate Ion Electrode for the Monitoring of the Electroreduction of Salicylic Acid

Abstract

An ion selective electrode is described for measuring the unreacted salicylate ion concentration during the electroreduction of salicylic acid. Conditions for making measurements are discussed.     

新型Schiff碱双核铜(Ⅱ)配合物为载体的水杨酸根离子电极的研究

研究了5-溴水杨醛缩三乙烯四胺双核铜(Ⅱ)配合物为载体的高选择性水杨酸根离子中性膜电极。该电极对水杨酸根离子(Sal-)具有优良的电位响应特性并呈现出反Hofmeister选择性行为,其选择性次序为:Sal-ClO4-SCN-I-NO3-Br-SO42-Ac-NO2-Cl-SO23-。电极在pH=5.0的磷酸盐缓冲体系中,与Sal-在4.0×10-6～1.0×10-1mol/L浓度范围内呈近能斯特响应,斜率为58.0mV/dec(28℃),检出限为1.0×10-6mol/L。采用紫外可见光谱技术研究了电极响应机理。将该电极应用于药品分析,结果令人满意。     

Ion chromatographic determination of salicylate in human serum with a bulk acoustic wave sensor as detector

Salicylate is a hydrolysis product of salicylate-containing drugs (such as aspirin) in patients' blood. Monitoring of this ion in blood is helpful for diagnosing of overdosage of these drugs. The present paper describes an ion chromatography (IC) method developed for determination of total salicylate in human serum, in which a hulk acoustic wave (BAW) sensor was used as detector; 0.5 mmoI/L sodium carbonate (Na₂CO₃, pH 8.5) served as mobile phase. Interference in the determination was negligible. The method is simple, rapid, accurate, and precise. Serum salicylate was analyzed using both the proposed IC-BAW method and the classical Trinder spec-trophotometric method, and the results showed that the two method agreed well.     

Bis (trans-cinnamaldehyde) ethylene diimine dibromonickel (II) complex as a neutral carrier for salicylate-selective liquid membrane and coated graphite sensors

A salicylate PVC-based membrane (SPME) and a coated graphite membrane (SCGE) electrodes by using a new tetracoordinate organonickel complex as ion carrier were prepared. Both sensors show a Nernstian response to salicylate ions over a very wide concentration ranges (1.0×10⁻⁵-1.0×10⁻¹ M for SPME and 1.0×10⁻⁶-1.0×10⁻² M for SCGE) in the pH of 7.0. The best selectivities were obtained for the membrane incorporating 30% PVC, 63% plasticizer, 2% cationic additive and 5% ionophore. The electrodes possess satisfactory reproducibility, very short response time (∼10 s) in the whole concentration ranges, and excellent discriminating ability for salicylate ions with respect to the most common organic and inorganic anions. The detection limits of proposed sensors are 5.0×10⁻⁶ and 7.0×10⁻⁷ M for SPME and SCGE, respectively. The electrodes were successfully used for determination of salicylate in biological samples.