四苯硼钠法测定吡哌酸含量

介绍一种测定吡哌酸含量的有效方法。在ｐＨ＝３．６的ＨＡｃ－ＮａＡｃ缓冲溶液中,吡哌酸与四苯硼钠可形成１：１的定量沉淀,待沉淀反应完全后,以溴酚蓝为指示剂,用烃铵盐标准溶液回滴过量的四苯硼钠,方法简便、快速,应用于吡哌酸原料药品测定,其回收率为９９．４４％～１００．０９％,最大相对误差〈±０．６％,与药典法测得的结果基本一致。     

氯化亚铜中亚铜及高价铜盐含量的示波滴定

１引言氯化亚铜含量的测定在国家标准分析方法中是根据亚铜离子能使Ｆｅ３＋还原为Ｆｅ２＋，然后以邻菲啉－硫酸亚铁络合物作指示剂用高铈盐进行滴定。氯化亚铜中高价铜盐测定则利用高价铜盐能溶于５ｍｏｌ／Ｌ乙酸．而亚铜盐不能溶解进行分离，然后再用碘量法进行测定，手续十分麻烦。本文根据ＣＵ（Ⅰ）与四苯硼钠定量生成沉淀，用示波滴定法中的四苯硼钠法进行氯化亚铜含量的测定，高价铜盐被抗坏血酸还原，再用四苯硼钠法进行滴定，差量法计算出高价铜盐含量，操作简便，终点直观，测定结果准确。２实验部分２．１主要仪器与试剂ＬＳ－…     

铜合金中铜的示波滴定—四苯硼钠法

本文报道了铜合金中铜的示波滴定方法。样品酸溶后，用抗坏血酸还的Ｃｕ＾２＋为Ｃｕ＾＋，加入过量的四苯硼钠，在ＰＨ５－６的ＨＡｃ－ＮａＡｃ缓冲溶液中，定量形成Ｃｕ－ＴＰＢ沉淀，过量的ＴＰＢ＾－，以Ｔｌ＾＋标准溶液进行示波滴定，铜合金中共存元素不干扰测定。铜的测定回收率９９．８％－１００．１％。进行了多种铜合金中铜含量的测定，结果令人满意。     

间接原子发射光谱法测定氢溴酸山莨菪碱

研究了电感耦合等离子体-原子发射光谱法间接测定氢溴酸山莨菪碱。在pH5．0溶液中过量四苯硼钠可使氢溴酸山莨菪碱沉淀完全，加入氯化钾沉淀滤液中剩余的四苯硼钠，测定滤液中过量的钾，可以计算得到氢溴酸山莨菪碱的含量。方法简单快速，回收率在97％～102％之间，相对标准偏差为1．3％。     

电导滴定法快速测定钾的含量

１引言测定钾的含量常用火焰光度法和四苯硼钠重量法，火焰光度法适用于微量分析，四苯硼钠重量法的测定周期长。电导滴定法用于测定一些可发生沉淀反应的离子时，具有快速简便的优点。本文采用四苯硼钠溶液滴定，电导滴定法测定高、中含量组分钾的含量，测定周期仅需１０ｍｉｎ，所用试剂量少，不受样品中水不溶物的干扰，适用于钾盐、卤水和复合肥中钾的测定。２实验部分２．１仪器和药品电导率的测定采用ＤＤＳ－１２Ａ型数字式电导率仪和２１６型电导电极。四苯硼钠（Ｎａ［Ｂ（６Ｈ５）４］）为分析纯试剂，配成水溶液后用基准ＫＣＩ标…     

间接原子发射光谱法测定碘解磷定

研究了等离子发射光谱法间接测定碘解磷定。在pH5．0的溶液中，当四苯硼钠过量时可完全沉淀碘解磷定，在滤液中加入过量的氯化钾沉淀剩余的四苯硼钠，再测定滤液中过量的钾，可以计算得到碘解磷定的含量。方法简单快速，回收率在96％～102％之间，相对标准偏差为1．7％。     

聚苯胺／聚乙烯醇载体尼古丁膜电极的研究

聚苯胺／聚乙烯醇复合物与四苯硼钠－尼古丁混合，制成尼古丁膜电极，在ｐＨ＝２～７电极时１０＾－２～１０＾－５ｍｏｌ／Ｌ的尼古丁有良好的线性响应，检测下限可达４．０×１０＾－６ｍｏｌ／Ｌ。用于烟草样品中尼古丁含量的测定，平均回收率为９８．４％，相对标准偏差为０．９３％，与紫外分光光度法对比，结果令人满意。     

示波极谱滴定法用于药物制剂中扑尔敏的测定

扑尔敏是感冒药中常有的一种组分,其测定方法有分光光度法和毛细管电泳法,电分析方法还未见报道。本文根据四苯硼钠与扑尔敏在一定条件下能定量形成沉淀,沉淀经过滤洗涤后,滤液以汞膜电极为指示电极,钨电极为参比电极,在碱性底液中用四乙基氯化铵标准溶液返滴过量的Na-TPB,利用示波极谱图上TPB切口消失指示滴定终点,差量法计算样品含量。该法终点直观,手续简便,灵敏准确,对速效伤风胶囊和思普诺儿童伤风素中扑尔敏进行分析测定,获得满意结果。     

示波滴定法测定铝合金中铜的含量

研究了铝合金中铜含量的示波滴定法。在酸性溶液中抗坏血酸将铜（Ⅱ）还原为铜（Ⅰ）,用过量四苯硼钠沉淀铜（Ⅰ）,过量的四苯硼钠用氯化四乙基铵标准溶液返滴定,以四苯硼钠切口消失为终点,计算出铜含量。方法终点变化敏锐,不外加指示剂,与标准分析方法相比较,操作简便、快速,所用分析试剂无毒,测定结果的RSD小于0．19％,标准加入回收率为98．7％～102．0％。     

原子吸收光谱法间接测定碘解磷定

研究了原子吸收光谱法间接测定碘解磷定。在pH5．0溶液中,当四苯硼钠过量时可完全沉淀碘解磷定,在滤液中加入过量的KCl沉淀剩余的四苯硼钠．再测定滤液中的过量的钾,可以计算得到碘解磷定的量。方法的回收率在98％～103％之间．相对标准偏差为1．8％。     

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%.     

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.     

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.     

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.     

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.     

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.     

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.