聚氯乙烯膜氧氟沙星和曲马多选择电极的研制与应用

报道了以氧氟沙星碘化物与碘化铋的分子缔合物为电活性物的新型聚氯乙烯膜氧氟沙星选择电极。并以类似的方法报道了曲马多选择电极。氧氟沙星电极的特响应范围为１．０×１０＾－２－２．２×１０＾－５ｍｏｌ／Ｌ，斜率为３０ｍＶ／ＰＣ，检测限为１．６×１０＾－５ｍｏｌ／Ｌ。     

簇合物膜亚硫酸根离子选择性电极的研制

报道了复ＭｏＳ６２－４在铜表面形成不溶性族合物膜的性质，研制了一种簇合物膜亚硫酸根离子选择电极。电极对ＨＳＯ＾－３的线性响应范围为１×１０＾－４－１×１０＾－１ｍｏｌ／Ｌ；检测限为８×１０＾－５ｍｏｌ／Ｌ；响应斜度为５８．５ｍＶ／ｄｅｃ；适宜的ｐＨ范围为９－１０。     

全固态林可霉素选择电极的研制及应用

本以石墨棒为导电基体，以硅钨酸，林可霉素为电活性和的制成了全固态林可霉素离子选择电极。所制电极在１．０×１０＾－１－５．０×１０＾－５ｍｏｌ／Ｌ浓度范围内有线性响应，斜率为５８．３ｍＶ／ｐＣ，检测下限为２．５×１０＾－５ｍｏｌ／Ｌ。电极响应迅速，具有良好的稳定性，可用于林可霉素含量的快速测定。     

铁的单点络合滴定法研究

本研究了Ｆｅ＾３＋的单点络合滴定法，导出了定量关系式，比较了以铂电极为指示电极和以ＰＶＣ膜四氯络铁（Ⅲ）阴离子电极为指示电极时电位测量的稳定性及所得的分析结果。在Ｆｅ＾３＋浓度为１．０００×１０＾－３ｍｏｌ／Ｌ时，１８次实验的平均值为１．０２×１０＾－４ｍｏｌ／Ｌ，相对偏差小于１．７％；Ｆｅ＾３＋在５．０×１０＾３ｍｏｌ／Ｌ以上时，相对偏差小于０．１％；其浓度小于１０＾－３ｍｏｌ／Ｌ而大于５×１     

L—天冬门酰胺微生物电极的研制

以谷氨酸棒状杆菌作为生物催化剂，与基础氨气敏电极结合制成对Ｌ－天冬门酰胺响应的微生物电极，在３０℃时选择ＰＨ＝８．５的硼酸缓冲体系，测得电极的线性范围为７．１×１０＾－５－１．１×１０＾－２ｍｏｌ／Ｌ，斜率为５１．４ｍＶ／ｄｅｃ，检测下限为２．０×１０＾－５ｍｏｌ／Ｌ，响应时间为４－７ｍｉｎ寿命达３０ｄ以上。     

聚氯乙烯膜奎宁选择电极的研制与应用

本报道了一种以奎宁溴汞酸盐为电活性物的ＰＶＣ膜奎宁选择电极，其线性响应范围为１．０×１０＾－２－１．０×１０＾－６ｍｏｌ／Ｌ；级差５８±１ｍＶ；检测限为８．２×１０＾－７ｍｏｌ／Ｌ。以此电极测定奎宁的含量，方法简单、快速、结果与药典法相符。     

盐酸氟桂嗪离子选择性电极的制备及应用

研制了盐酸氟桂嗪离子选择性电极。利用正交设计法综合研究了活性的类型、含量以及增塑剂等因素对ＰＶＣ膜电极响应性能的影响，结果表明，以盐酸氟桂嗪－四苯硼钠离子缔合物为活性物质，ＤＢＰ或ＤＯＰ为增塑剂制成的ＰＶＣ膜电极的性能最佳。其响应范围为１．０×１０＾－４－５．０×１０＾－３ｍｏｌ／Ｌ，检测下限为３．５×１０＾５ｍｏｌ／Ｌ，响应斜率为５８ｍＶ（２５℃）。应用该电极对合成样品及胶囊样品中盐酸氟桂嗪含量     

洛美沙星离子选择电极的研制及应用

用正交设计法研究了离子缔合物的种类,膜相中活性物浓度和增塑剂３个因素对电极性能的影响,以四苯硼－洛美沙星形成的缔合物为电活性物质研制了涂碳ＰＶＣ膜洛美沙星电极。其能斯特响应范围为２．０×１０＾－３－１．０×１０＾－５ｍｏｌ／Ｌ;检测限为４．０×１０＾－６ｍｏｌ／Ｌ,级差为２８．９ｍＶ／ｐＣ。     

苄氧基甲基12—冠—3的合成与锂离子选择性电极研究

报道了苄氧基甲基－１２－冠－３－的合成，并以此化合物作载体研制成锂离子选择电极。用苄氧基甲基－１２冠－３－为载体的电极对锂离子响应拇性范围为１．０×１０＾－１－８．３×１０＾－５ｍｏｌ／Ｌ．检测限为４．２×１０＾－５ｍｏｌ／Ｌ，斜率为５７．４ｍＶ／ｐＬｉ。电极具有好的稳定性和重现性。     

阿霉素在钴离子注入修饰电极上的电化学行为及其应用

阿霉素在０．１ｍｏｌ／Ｌ ＨＡｃ－ＮａＡｃ（ｐＨ４．６２）缓冲溶液中用注入钴的修饰玻碳电极为工作电极进行伏安测定,得到一良好的还原峰;Ｅｐ＝－０．５２２Ｖ（ｖｓ．ＳＣＥ）。峰电流与阿霉素浓度在１．４×１０＾－６－１．４×１０＾－６ｍｏｌ／Ｌ和１．４×１０＾－６－５．６×１０＾－５ｍｏｌ／Ｌ范围内呈线性关系,。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

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%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

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.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

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.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

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.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

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.