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1.
Debendra K. Mohapatra Dhananjoy Mondal Mukund S. Chorghade Mukund K. Gurjar 《Tetrahedron letters》2006,47(52):9215-9219
The non-proteinogenic amino acid 3-hydroxy-4-methylproline (HMP) is an active constituent of some potent antimicrobials including echinocandins, nostopeptins, pneumocandins, sporiofungin and mulundocandins. A synthesis has been achieved in 10 steps with 29% overall yield; the Evans’ aldol reaction using Crimmins’ modified method was pivotal to the success of the strategy. 相似文献
2.
Emmanuel DardennesÁrpád Kovács-Kulyassa Andrea RenzettiJanos Sapi Jean-Yves Laronze 《Tetrahedron letters》2003,44(2):221-223
Chiral pyrano- and pyrrolidino-fused tryptamines were prepared by a diasteroselective trimolecular condensation between indole, Garner's aldehyde and Meldrum's acid, followed by selective functional group transformations. 相似文献
3.
The title compound is a bifunctional receptors including a thiourea group and a crown ether ring. Due to many possible potentials as a new class of reagents for membrane transports,ion-selective electrodes as well as reaction catalysts, the design and synthesis of bifunctional receptors for simultaneous binding of cations and anions is of ongoning interest in srprarnolecular chemistry1-5. In bifunctional receptors, the binding sites for anions and cations are covalently linked so as to exhibit allosteric or cooperative complexation where the binding affinity for anions(cations)is modified as a result of the cation(anion) complexation.Literature[6] reported that the ability of the thiourea group to bind anions is significantly enhanced when Na+ is bound to the crown moiety. To date, however only a few receptors of this class have been reported.6-8In this paper, we report an improved procedure under microwave irradiation that gives higher yields of title compound and needs fewer reaction times than traditional method.The structure of this compound was determined by IR ,element analysis and X-ray analysis.Scheme 1 The reaction equationThe crystal belongs to triclinic crystal system, P-1 space group, a=0.9547(0)nm, b=1.3637(3)nm,c=1.6029(3)nm, α =75.33(3) , β =83.62(3) , γ =70.99(3) ,Z=4,Dc=1.335g/cm3,F(000)=816,R1= 0.0557 ,wR2=0.1281. It is assembled into a three-dimensionalsupramolecule by intermolecular hydrogen bonds. 相似文献
4.
5.
This study demonstrates the separation of active ingredients in acne formulations (salicylic acid, cloramphenicol and resorcinol in presence of azulene) by capillary zone electrophoresis. Factors affecting their separations were the buffer pH and concentration, applied voltage, sample preparation, and presence of additives. Optimun results were obtained with a 50 mM sodium tetraborate-50 mM sodium phosphate, pH 9.0. The carrier electrolyte gave baseline separation with good resolution, short migration times (<6 min), great reproducibility and accuracy. Calibration plots were linear over at least three orders of magnitude of analyte concentrations, the lower limits of detection being within the range 0.39-1.25 μg ml−1. The procedure was fast and reliable and commercial pharmaceuticals could be analysed without prior sample clean-up procedure. 相似文献
6.
Sahadev R. K. Sharma S. K. Sindhwani 《Monatshefte für Chemie / Chemical Monthly》1992,123(10):883-889
Summary The chelation behaviour of some trivalent lanthanide and yttrium metal ion with biologically active 2-hydroxy-1-naphthaldehyde thiosemicarbazone (HNATS) has been investigated by potentiomotric measurements at 20±0.5°C in 75% (v/v) dioxane-water medium at various ionic strengths of sodium perchlorate. The method of Bjerrum and Calvin, as modified by Irving and Rossotti has been used to find out the values of
(average number of ligand bound per metal ion) andpL (free ligand exponent). The formation constants of metal chelates have been computed on a PC-XT computer, using a program patterned after that of Sullivan et al. to give
n
values using weighted least squares method. TheS
min
values (S
min
=2) have been calculated. The order of formation constants of chelates was found to be: La3+3+3+3+3+3+3+3+3+3+. The formation constants of the chelates formed have been correlated to size and ionization potentials of the metal ions.
Potentiometrische Untersuchungen der Komplexierungsgleichgewichte zwischen einigen trivalenten Metallionen und biologisch aktivem 2-Hydroxy-1-naphthaldehyd-thiosemicarbazon (HNATS)
Zusammenfassung Es wurde das Chelierungsverhalten einiger trivalenter Lanthanidenionen mit biologisch aktivem 2-Hydroxy-1-naphthaldehyd-thiosemicarbazon (HNATS) mittels potentiometrischer Messungen bei 20±0.5°C in 75% (v/v) Dioxan-Wasser bei verschiedener Ionenstärke an Natriumperchlorat untersucht. Die Methode nach Bjerrum und Calvin in der Modifikation nach Irving und Rossotti wurde zur Ermittlung der Werte (mittlere Anzahl an Liganden pro Metallion) undpL (Exponent an freiem Liganden) verwendet. Die Komplexbildungskonstanten wurden in Anlehnung an Sullivan et al. an einem PC-XT Computer errechnet. DieS min-Werte (S min=2) wurden ebenfalls bestimmt. Die Reihung der Chelatbildungskonstanten war: La3+相似文献3+ 3+ 3+ 3+ 3+ 3+ 3+ 3+ 3+. Die Bildungskonstanten sind mit der Größe und dem Ionisierungspotential der Metallionen zu korrelieren.
7.
糠醛缩氨基硫脲合镍配合物的合成、晶体结构及表征 总被引:1,自引:0,他引:1
合成了糠醛缩氨基硫脲的Ni(Ⅱ)单核配合物,通过红外光谱、紫外光谱、X射线单晶衍射和热重-差热分析等手段对其结构进行了表征.单晶结构解析结果表明,标题化合物属于三方晶系,R3-空间群,晶胞参数为:a=1.4097(1)nm,b=1.4097(1)nm,c=2.0952(2)nm,α=90°,β=90°,γ=120°,V=3.6059(4)nm3,Z=9,Dc=1.638Mg/m3,μ=1.488mm-1,F(000)=1818,R1=0.0231,wR2=0.0619.配合物中镍离子采用4配位的平面正方形配位构型,晶体堆积中通过分子间氢键形成三维网状结构. 相似文献
8.
9.
利用交替三线性分解算法(ATLD)与高效液相色谱法相结合,在色谱保留时间为0.662 8~0.949 5min(间隔1/150 min)、紫外吸收波长为268~332 nm(间隔2 nm)且在未知干扰物2,3-二羟基苯甲酸存在下,同时测定了水溶液中光谱及色谱严重重叠的水杨酸(SA)和龙胆酸(GA)的含量,回收率分别为(102.2±6.7)%,(102.1±4.1)%,分辨结果与实际结果一致。研究结果表明:该方法定量快速准确、实验操作步骤简单,说明ATLD算法收敛快速稳定,对复杂体系中组分数估计不敏感,能有效解决色谱中的二阶校正问题。 相似文献
10.