聚天冬氨酸铂的合成与表征

铂类化合物中顺铂、卡铂等目前已经应用于卵巢癌、睾丸癌等肿瘤疾患的治疗,然而这类药物在低剂量下也存在严重的毒副作用[1,2,3].     

丙氨酸铂配合物的合成与表征

顺铂、卡铂等铂配合物目前已经应用于卵巢癌、睾丸癌等肿瘤疾患的治疗,然而这类药物在低剂量下也存在严重的毒副作用,同时还存在溶解性差、不稳定等缺点[1,2,3].寻找高效、低毒的新一代铂类抗癌药物是医药领域的迫切任务.     

Synthesis and characterization of a platinum(II) complex with N-acetyl-L-cysteine

Synthesis and spectroscopic studies in the solid-state of a platinum(II) complex with N-acetyl-L-cysteine are described. Elemental analyses are consistent with composition Pt₂(C₅H₈NO₃S)₄ · 3H₂O. Solid-state ¹³C NMR, infrared, and U-Vis spectroscopic results are consistent with coordination of the ligand to platinum(II) through sulfur. Thermal analyses confirmed water in the complex composition. Final residue of the thermal treatment was identified by powder X-ray diffractometry as metallic platinum.     

Synthesis and characterization of a platinum(II) complex of camphenylphosphonic acid

Camphenylphosphonic acid RPO₃H₂, prepared by the literature reaction of PCl₅ with camphene, has been characterized by a single-crystal X-ray diffraction study. The compound crystallizes with a double chain structure formed by connected eight-membered hydrogen-bonded rings. Reaction of RPO₃H₂ with cis-[PtCl₂(PPh₃)₂] and excess silver(I) oxide in refluxing dichloromethane gives the platinum(II) phosphonate complex [Pt{O₃PR}(PPh₃)₂]. ³¹P{¹H} NMR spectroscopic characterization of [Pt{O₃PR}(PPh₃)₂] shows that the two PPh₃ ligands are inequivalent due to asymmetry of the camphenyl group. An X-ray diffraction study on the platinum complex shows that the PC–H bond is directed toward the four-membered ring, resulting in the terpene group pointing away from the ring, in contrast to the previously reported structure of the saturated camphanylphosphonate complex. The differences are discussed in terms of steric interactions involving the phosphonate ligands.     

Synthesis and characterization of a new platinum(II) complex with L-mimosine

Synthesis and characterization of a new Pt(II)–mimosine complex are described. Elemental, mass spectrometry and thermal analyses for the complex are consistent with the formula [PtCl₂(C₈H₁₀N₂O₄)]·1.5H₂O. ¹³C NMR, ¹⁵N NMR and infrared spectroscopy indicate coordination of the ligand to Pt(II) through the N and O atoms in a square-planar geometry. The final residue after thermal treatment was identified as metallic Pt. The complex is soluble in dimethylsulfoxide.     

The preparation and reactions of a π-bound organic isoselenocyanate complex of platinum: Formation of an η2-diselenocarbonimidato complex

Reaction of Pt(Ph₃P)₂C₂H₄ with p-tolyl isoselenocyanate yields the first known example of a π-bound organic isoselenocyanate ligand in the complex Pt(η²-SeCNC₇H₇)(Ph₃P)₂. Reaction of this complex with methyl iodide results in alkylation at the selenium atom rather than at nitrogen, with resultant loss of selenium to yield PtI₂(CNC₇H₇)(Ph₃P) as the final product. If the reaction of Pt(Ph₃P)₂C₂H₄ with p-tolyl isoselenocyanate is carried out in CH₂Cl₂ solution, selenium abstraction occurs and the complex Pt(η²-Se₂CNC₇H₇)-(CNC₇H₇)(Ph₃P) is formed which contains both an isonitrile ligand and the as yet unreported diselenocarbonimidato ligand. Alkylation of this ligand failed to yield a diselenocarbamate complex.     

Crown ether complex cation ionic liquids: preparation and applications in organic reactions

A series of crown ether complex cation ionic liquids (CECILs) were designed, synthesised and characterised by NMR spectroscopy, HRMS, thermogravimetric differential thermal analysis (TG-DTA) and elemental analysis. Their applications in various organic reactions were investigated: [15-C-5Na][OH], [15-C-5Na][OAc], [18-C-6K][OH] and [18-C-6K][OAc] (15-C-5=[15]crown-5; 18-C-6=[18]crown-6) efficiently catalysed the Michael addition of alkenes and relevant nucleophiles; [18-C-6K][OH] and [15-C-5Na][OH] effectively catalysed the Henry reaction of nitromethane and aromatic aldehydes; [18-C-6K][OH] has excellent catalytic efficiency for Knoevenagel condensation of aromatic aldehydes and malononitrile; PdCl(2) /[18-C-6K](3)[PO(4)]/K(2)CO(3) efficaciously catalysed the Heck reaction of olefins and aromatic halides; [18-C-6K][BrO(3)] can be used as both oxidant and solvent in the oxidation reaction of aromatic alcohols. The CECIL catalysts [15-C-5Na][OH] (Michael addition) and [18-C-6K][OH] (Henry reaction) can be recycled and reused several times without obvious loss of activity and their recovery is very simple.     

Synthesis,characterization and optical properties of a new cationic cyclometalated platinum(ii) complex

The cyclometalated platinum (II) complex, [Pt(ppy)(ppyH)₂] OTF, 2 , in which ppy and ppyH denote the cyclometalated and non‐cyclometalated 2‐phenylpyridine ligand respectively, was prepared from the reaction of the platinum(IV) complex [PtMe₃(OTF)], 1 , with 3 equiv 2‐phenylpyridine at room temperature. The cyclometalated complex 2 was characterized using ¹H NMR spectroscopy. The solid state structure of 2 was further identified by single crystal X‐ray structure determination. 2 displays a green emission in solution and in solid state at room temperature and TD‐DFT calculations is used to elucidate the origin of the electronic transitions in the UV–vis spectrum of 2 .     

Isomerization of light alkanes: preparation and characterization of platinum promoted sulfated zirconia catalysts

Summary Platinum-promoted sulfated zirconia catalysts active in n-hexane isomerization were prepared in a one-step synthesis and characterized. The crystallinity and sulfur contents depend mainly on the calcination temperature. The stability of the sulphate in the presence of hydrogen is reduced by the presence of Pt.     

Synthesis,characterization and initial biological studies of a new platinum(II) complex with deoxyalliin

A new platinum(II) complex with deoxyalliin was synthesized and characterized by chemical and spectroscopic techniques. Elemental and mass spectrometry analyses of the solid complex fit to the composition [Pt(C₆H₁₁NO₂S)Cl₂]·H₂O. ¹³C NMR, ¹⁵N NMR and infrared spectra of the complex are consistent with coordination of deoxyalliin to Pt(II) through the nitrogen and sulfur atoms forming a square-planar geometry. The complex is soluble in dimethylsulfoxide. Biological analysis for evaluation of a potential cytotoxic effect of the complex was performed using HeLa cells, a human cervix adenocarcinoma-derived cell line. The results were compared with those of a palladium(II) complex previously described.     

Multiple hydrogen bondings in a platinum complex

An unprecedented example of a platinum(II) complex with simultaneous formation of intermolecular NH···I-Pt and CH···I-Pt H-bondings (with neighboring platinum center) and an intramolecular CH···Pt hydrogen bonding in solid state is described. There are indications showing that the complex in solution probably forms a different kind of H-bonding type interaction.     

The preparation of chloroplatinic acid labelled with platinum radioisotopes

A procedure has been worked out for the preparation of chloroplatinic acid from natural metallic platinum irradiated in a nuclear reactor and purified from¹⁹⁹Au impurities by extraction from acidic solutions with ethyl acetate. It was shown that the effective K X-ray activity of natural platinum on irradiation with moderate neutron fluxes /3×10¹³/ was comparable with that of^195mPt obtained from 100%¹⁹⁴Pt/with identical neutron fluxes/. Contaminations from¹⁹³Pt /50 years/ is insignificant and do not produce noticeable radiation loads on the organism on medical tests in vivo.     

Dioxygen activation by an osmium-dihydride: preparation and characterization of a d4 square-planar complex

Exposure of OsH2Cl2(PiPr3)2 to air or bubbling with pure O2 affords the dioxo-Os(VI) compound OsO2Cl2(PiPr3)2 as result of a direct O=O double bond activation reaction. This Os(VI) species is reduced in the presence of n-BuLi to the novel dioxo-Os(IV) derivative OsO2(PiPr3)2, a rare example of a d4 square-planar compound.     

Novel species of soluble thermally stable poly(keto ether ether amide)s: preparation,characterization, and properties

A new diamine containing one keto and four ether groups was prepared through a three‐step reaction: first, hydroquinone was reacted with 1‐fluoro‐4‐nitrobenzene and 4‐(4‐nitrophenoxy) phenol was obtained. The next step was reduction of nitro group to amino group in which 4‐(4‐aminophenoxy) phenol was prepared. In the final step, the new diamine named as bis(4‐(4‐(4‐aminophenoxy)phenoxy)phenyl) methanone was synthesized through reaction of the later compound with 4,4′‐difluoro benzophenone. All prepared materials were fully characterized by spectroscopic methods and elemental analysis. Novel species of poly(keto ether ether amide)s were synthesized via polymerization reaction of the diamine with different diacid chlorides including terephthaloyl chloride, isophthaloyl chloride, and adipoyl chloride. All polyamides were characterized, and their properties such as thermal behavior, thermal stability, solubility, viscosity, water uptake, and crystallinity were investigated and compared together. The glass transition temperatures of the polymers were about 204–232°C, and their 10% weight losses were in the range of 396–448°C. Polymers showed high thermal stability and enhanced solubility that mainly resulted from incorporation of the diamine structure containing keto, ether, and aromatic units into polyamide backbones. Copyright © 2014 John Wiley & Sons, Ltd.     

The x-ray structure of a five-coordinate platinum(II) complex cation

[NEt₄][W₂(CO)₁₀SC₆Cl₅] has been synthesised via the mononuclear pentacarbonyl species and characterised by elemental, IR and X-ray analyses; the bridging W-S-W angle in the dinuclear anion is 132.1°     

醇醚糖苷的制备及其复配性能研究

用环氧乙烷(EO)平均加合数分别为0.8和3.0的脂肪醇醚AEO0.8、AEO3.0为原料,直接与葡萄糖反应,反应混合物用超临界CO2萃取技术提纯,分别得到醇醚糖苷AEG08、AEG30,并用气相色谱法定量分析了AEG08和AEG30的组成.然后分别对AEG08、AEG30与醇醚硫酸盐(AES)及十二烷基甜菜碱(BS-12)复配体系的表面张力、临界胶束浓度(cmc)、润湿力、乳化力、起泡及泡沫稳定性进行了测定.结果表明AEG与AES按不同质量比复配后,表面张力、cmc、起泡及泡沫稳定性显示了一定的协同效应,润湿力和乳化力显示了负的协同效应;而AEG与BS-12复配后,其表面张力、cmc、润湿力、乳化力、起泡及泡沫稳定性都显示了明显的协同效应.     

The bis-barium complex of a butterfly crown ether as a phototunable supramolecular catalyst

Reversible phototuning of the catalytic efficiency of the bis-barium complex of azobis(benzo-18-crown-6) in the basic ethanolysis of anilide derivatives has been achieved by light-induced cis right arrow over left arrow trans interconversion of the azobenzene spacer unit of the catalyst. The geometry of the productive catalyst-substrate complex is more favorable when the concave cis form of the catalyst is involved. Continuous photoregulation of the catalytic activity at any intermediate value between the "HIGH" and "LOW" levels was achieved by proper adjustment of the excitation wavelength or the irradiation time. The complete and relatively fast interconvertibility of photostationary states allowed the activity of the catalyst to be repeatedly photoswitched "HIGH" and "LOW" in the course of the same run.