硫酸颜色反应用于荧光法测定利血平研究

提出了硫酸颜色反应用于利血平的荧光分析新方法。利用血平与浓硫酸反应，生成强荧光物质，所得产物的荧光强度与利血平的浓度在０－０．６μｇ／ｍＬ范围内有良好的线性关系。检测限为０．２ｎｇ／ｍＬ。本法可直接用于尿液中利血平的定量分析，回收率为８２．５％－８４．２％。     

催化光度法测定痕量敌百虫

以过氧化氢－联苯胺为指示反应，在檬檬钠弱碱性介质中建立了催化光度测定痕量敌百虫亲方法。方法灵敏度为０．０５４ｍｇ／Ｌ，线性范围为０－２８．８ｍｇ／Ｌ，应用于痕量敌百虫试样的快速分析，结果满意。     

荧光法测定环境水中微量久效磷

采用荧光分光光度法测定了环境水中微量久效磷的含量。在０．２５％的吲哚丙酮溶液与０．２５％的过硼酸钠溶液的混合液中，体系温度为５℃时，λｅｘ／λｅｍ＝４２０ｎｍ／５００ｎｍ，检测限为４．０μｇ／Ｌ，线性范围为０－３．２μｇ／ｍＬ，回收率为９８％－１０４％，结果令人满意。     

光化学荧光分析法测定头孢氨苄的研究

在ｐＨ４．０的缓冲溶液中，头孢氨苄在紫外光照射下能发生光化学反应，形成具有荧光的产物，λｅｘ为３４５ｎｍ，λｅｍ为４３２ｎｍ。在头孢氨苄浓度为０．１－４．０μｇ／ｍｌ范围内，荧光强度与浓度呈良好的线性关系，由此建立了头孢氨苄的光化学荧光测定法。方法的检出限为０．０１μｇ／ｍｌ，相对标准偏差为０．９３％。本法简便，快速且灵敏度高，可用于尿液中头孢氨苄含量的测定。     

流动注射停流荧光动力学分析法测定痕量铁的研究

利用自行组装的流动注射停流荧光动力学分析装置，研究了铁（Ⅲ）与３，５－二溴水杨基荧光酮的荧光动力学反应性质，提出了一种快速，简便，精确地测定痕量铁的新方法，其线性范围为０．０２０－０．２５０μｇ／ｍＬ，线性相关系数为０．９９９，检测限为１０ｎｇ／ｍＬ，以０．２００μｇ／ｍＬ的铁（Ⅲ）作精度试验，Ｒ．Ｓ．Ｄ％＝２．１％（ｎ＝１１）。该方法已成功地用于铝合金及桃树叶中痕量铁的测定，结果分别与ＩＣＰ法和     

镧、轧、镥、钇和钪与铽-乙酰水杨酸共发荧光体系的研究和应用

研究发现，镧、轧、镥、钇和钪５种稀土离子可以分别与铽－乙酰基水杨酸形成优良的 共发荧光体系。在最佳条件下，５种离子可分别使铽－乙酰水杨酸体系的荧光增强３５０、５８、 １０８、７３和４０倍。分别研究了各共发光体系的形成条件、荧光特点和影响因素。利用铽－镧－乙 酰水杨酸体系，可使铽的检测限降到３．０×１０－１０ｍｏｌ／Ｌ，铽浓度在５．０×１０－９～３．０×１０－６　ｍｏｌ／Ｌ 范围内与荧光强度呈线性关系。应用于稀土合成样品和包头稀土标准氧化物中的铽的测定， 结果满意。回收试验的回收率为９３％±４．２％。分析各体系后，对共发荧光的机理进行了初 步的探讨。     

同步荧光法测定复方新诺明中磺胺甲基异恶唑和甲氧苄氨嘧啶的含量…

本文采用同步荧光技术对复方新诺明中有效成份磺胺甲基异恶唑和甲氧苄氨嘧啶进行测定，在△λ分别为７２ｎｍ和９４ｎｍ的条件下，测定样品中所含有效成份相当于标示量的９５．１２％－１０５．６８％；回收率为９５．５％－９８．１％；线性范围磺胺甲基异恶唑为０．１２５－４．００μｇ／ｍｌ。甲氧苄氨嘧啶为０．１２５－３．００μｇ／ｍｌ；相关系数分别为０．９９７６和０．９９６８。不经分离和掩蔽直接连续测定，效果良好。     

荧光光度法测定环境水中微量甲基对硫磷

研究了荧光分光光度法测定环境水中甲基对硫磷的一。在吲哚丙酮溶液０．２５％，过硼酸钠溶液０．２５％溶液中，温度５℃、λｅｘ／λｅｍ＝４１０ｎｍ／４９０ｎｍ，检出限５．０（５．２）μｇ／Ｌ，线性范围０－２．０（２．６）ｍｇ／Ｌ，回收率达９８－１０２％，结果满意。     

流动注射—胶束荧光法快速测定葡萄糖中的微量铝

本提出Ａｌ－Ｃａｌｃｅｉｎ－ＣＴＭＡＢ－Ｔｗｅｅｎ－８０体系，用流动注射－胶束荧光法快速测定葡萄糖中微量铝的方法。荧光最大激发波长和发射波长分别为４７８．０和５０９．０ｎｍ．Ａｌ＾３＋的浓度在０－６μｇ／ｍＬ范围内标准曲线呈线性关系，方法检出下限为８．４２×１０＾－３μ／ｍＬ。方法已用于测定葡萄糖中微量铝，相对标准偏差为１％左右，回收率为９５－１０１％，进样频率为１４０次／ｈ，进样量为０．４４３     

荧光分析法测定痕量丁二酮

本文报道了邻苯二胺与丁二酮在１ｍｏｌ／ＬＨ２ＳＯ４介质中反应生成２，３－二甲基喹喔啉。该化合物具有较强的荧光（λｘ／λｅｍ＝３４０ｎｍ／４９０ｎｍ）其荧光量子产率ΦＦ＝０．１０１。丁二酮浓度在４．０×１０＾－７～５．２×１０＾－５ｍｏｌ／Ｌ范围内与转化成产物的相对荧光强度呈线性关系，相对标准偏差为１％，检出限为１．３×１０＾－７ｍｏｌ／Ｌ，考察了３０种物质表明，该法选择性好，用于实际啤酒样品中丁二     

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.     

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.     

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.     

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.