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本文比较了Mo(Ⅵ)-1-(2-吡啶基偶氮)-2-萘酚(PAN)与Mo(Ⅵ)-4(2-吡啶基偶氮)间苯二酚(PAR)的极谱性质,讨论它们在作为吸附波试剂时的优缺点,以求得在选择络合剂时的感性和理性认识.本文还报道了Mo(Ⅵ)-PAN-KBrO3吸附催化波体系,最佳实验条件,0.1mol/LHAc--NaAc,pH=4.6,0.01mol/LKBrO3,2.5×10-5mol/LPAN.峰电位为-0.71V(vs.SCE),检出限1×10-9mol/L,线性范围0~6×10-7mol/L 相似文献
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吡哆醛的电化学行为研究 总被引:2,自引:0,他引:2
用单扫示波极谱法,吡哆醛在0.2mol/LKCl+0.02mol/L naOH底液中,产生一良好的寺阶导数峰,EP=-1.30±0.01V(SCE),其峰高与浓度在2×10^-7-2×10^-4mol/L范围内成线性关系,检出限为1×10^-7mol/L实验证明,其电极过程为伴有微弱吸附性质的的可逆扩散过程(n=2),不在弱酸性和中性介质中时,吡哆醛的电极过程为前行动力学过程,其电极反应机理为伴有 相似文献
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铜(Ⅱ)锌(Ⅱ)—氟哌酸体系电化学行为及示波极谱法研究 总被引:1,自引:0,他引:1
铜(Ⅱ)和锌(Ⅱ)分别在0.1mol/LKH2PO4-Na2HPO4缓冲溶液(pH6.5)和0.25mol/LNH4Cl溶液中,与氟哌酸形成良好的络合吸附波,峰电位分别为-0.26V和-1.28V(vs.SCE),络合比分别为1:3和1:2,峰电流与铜(Ⅱ)和锌(Ⅱ)的浓度均在4.0×10^-7~5.0×10^-6nol/L范围内呈线性关系,检测限分别为7.0×10^-8和5.0×10^-8mol 相似文献
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将聚苯乙烯(PS)和乙基纤维素(EC)溶于CH_2Cl_2中,利用水中干燥法制备PS-EC复合膜微胶囊。当复合膜的微孔中含有磷酸三丁酯(TBP)时,微胶囊膜对Cr_2O_7~(2-)具有传输功能。芯材采用高浓度NaOH时,可使Cr_2O_7~(2-)逆浓差传输。研究了PS和EC的比例、微胶囊粒径、NaOH浓度及TBP含量对传输的影响.在适当条件下,10min内Cr_2O_7~(2-)的浓度由1×10~(-4)mol/L降至1×10~(-7)mol/L以下。 相似文献
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氧氟沙星的单扫描示波极谱分析 总被引:8,自引:0,他引:8
报道了一种灵敏的氧氟沙星测定方法-一阶导数单扫示波极谱分析,同时研究了它的极谱波性质和电极反应机理,在pH6.0的KH2PO4-Na2HPO4(PBS)底液中,氧氟沙星产生一个灵敏的还原峰,Ep=-1.55V(vs.SCE),其导数峰高与浓度在1.0×10^-5~4.6×10^-7mol/L范围内呈良好的线性关系,相关系数r=0.9996,检测下限为2.4×10^-7mol/L,可用于氧氟沙星片剂 相似文献
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聚N,N-双水杨醛乙二胺合钴修饰超微电极的制备及其在一氧化氮测定中应用的研究 总被引:6,自引:0,他引:6
通过电化学聚合法制备了聚N,N-双水杨醛乙二胺合钴[polyCo(Salen)]修饰超微电极,研究了该修饰电极的电催化性质及其在一氧化氮(NO)测定中的应用.实验结果表明,polyCo(Salen)修饰超微电极对NO的测定有高的灵敏度,NO的浓度在2.0×10-8~2.8×10-6mol/L范围内,电流与浓度呈良好的线性关系,线性相关系数为0.9998,检出限为1.0×10-8mol/L;该电极进一步修饰Nafion后,生物体中常见的物质如抗坏血酸、儿茶酚胺类神经递质的代谢物、NO的氧化产物NO-2等不干扰测定.本传感器可以满足NO在体分析的需要. 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular SN2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献