用色谱—质谱和质量以谱研究苯甲酸钐热分解反应

为合成某些芳香族有机化合物提供一种新途径，用色谱－质谱联用技术和质量色谱法研究了苯甲酸钐的热分解反应产物。其热分解产物溶入丙酮后有大量９，１０－蒽醌析出，其丙酮溶液中还含有１，２－二苯甲酰基苯（２５．６％）、苯甲酸（１８．７％）、二苯酮（１４．４％）、９－勿酮（８．２％）、９－苯甲勿（４．９％）、取苯（３．６％）、二苯甲烷（２．３％）、３－甲酰苯基联苯（２．１％）、二苯基乙二酮（１．９％）、４－甲     

毛细管电泳定量分析植物激素

详细研究了三种重要植物激素,生长素吲哚－３－乙酸,吲哚－３－丁酸,赤霉素ＧＡ３,ＧＡ４及激动素６－苄氨基嘌呤的毛细管电泳分离条件;１０ｍｉｎ内完成上述５组分分离;分离效率为５×１０＾５￣２．６×１０＾６,５组分检出限为４．５￣１８ｍｇ／Ｌ;迁移时间与峰高定量精度分别低于１．２％和２．４％,方法已用于香蕉叶中激素的测定。     

SDM—1型耐硫催化剂甲烷化反应动力学：II.宏观动力学模型

本文以工业应用为目的，采用内循环无梯度反应器，在５７３－６７３Ｋ，０．３０－１．２０ＭＰａ的条件下，原料气组成为Ｈ２ ５０－５４％，ＣＯ１１．７－２０．７％，ＣＨ４ ２．１－１４．３％，ＣＯ２ ６．４－１１．５％，Ｎ２ １２．２－１８．１％范围内，研究了φ×３ｍｍＳＤＭ－１型城市煤气耐硫甲烷化催化剂的宏观动力学方程选择 ＣＯ＋３Ｈ２＝ＣＨ４＋Ｈ２Ｏ （１） ＣＯ＋Ｈ２Ｏ＝ＣＯ２＋Ｈ２ （２）     

极谱法测定地质样品中痕量氯

提出了０．１％ＨＣＯＯＨ－８×１０＾３％百时香酚兰，－０．４ｍｏｌ／ＬＨＣｌＯ４－０．４％ＴｒｉｔｏｎＸ－１００极谱法痕量氯离子的新体系，检出限为０．１８μｇ／ｇ，ＲＳＤ为７．６％，标准样品测定结果与推荐值相吻合。     

天然气和二氧化碳转化制合成气的研究：Ⅵ Ni／Al2O3催化剂再生的疏…

采用γ－Ａｌ２Ｏ３为载体，以硝酸镍，硝酸镁和稀土硝酸盐为原料，按常规浸渍法制备负载型催化剂，其中Ｎｉ含量为９．１７％，助剂ＲＥ２Ｏ３和Ｍｇ含量分别为５．１８％和１．８０％。该催化剂简称为Ｎ－５－ＲＭ。催化反应评价采用双套管石英反应器，在多功能固定床流动反应装置上进行。     

对土壤及玉米植株中均三氮苯类除草剂的残留分析

土壤或玉米植株样品用Ｖ（甲醇）∶Ｖ（乙腈）＝１∶１提取,提取液用石油醚净化后,浓缩液过Ｃ１８小柱净化,最后用Ｎｏｖａ－ＰａｋＣ１８柱进行ＨＰＬＣ分析。回收率：氰草津为８２．４％～９９．８％,莠去津为８５．６％～１０２．３％,西草净为８９．１％～１０８．４％。     

牛颌下腺粘蛋白中糖组成的毛细管气相色谱分析

根据各种糖革键稳定性的差异，采用没的酸解方法，使各种单糖从牛颌下腺粘蛋白上游离下来。纯化后衍生成三甲基硅醚或糖醇乙酸酯，应用毛细管气相色谱技术分析。结果表明，牛颌下腺粘蛋白中含三类糖，即唾液酸、中性糖和氨基糖。每咱单糖的含量分别为５－Ｎ－乙酰神经氨酸４．３％；５－Ｎ＝乙醇酰神经氨酸１９．０％；岩藻糖３．２％；半乳糖５．１％；Ｎ－乙酰氨基半乳糖１８．４％；Ｎ－乙酰氨基葡萄糖８．７％。     

相转移催化酯化反相高效液相色谱法测定食品中有机酸

在不预分离水相中有机酸的情况下，用α－溴苯乙酮作酯化试剂，以１８－冠醚－６作相转移催化剂直接酯化有机酸，酯化液直接用高效液相色谱分析，紫外检测器检测，操作简便、干扰小、变异系数ＣＶ％＝１．４－５．６％检测下限５－２０μｇ／Ｌ，实际样品回收率９０．９－１０３．３％。     

高效液相色谱法测定人血浆中甲磺酸培氟沙星浓度

建立了一种测定人血浆中甲磺酸培氟沙星的匠相液相色谱方法,用的是ＺｏｒｂａｘＯＤＳＣ＿（１８）柱和用三乙醇胺调节成ｐＨ为３．０的甲醇－０．０４ｍｏｌ／ＬＨ＿３ＰＯ＿４溶液（８０：２０,Ｖ／Ｖ）的流动相,检测在２７６ｎｍ处进行,流量为１ｍＬ／ｍｉｎ,线性范围是６．０１×１０￣（－８）～３．０１×１０￣（－５）ｍｏｌ／Ｌ（γ＝０．９９９８）,检测极限为６．０１×１０￣（－８）ｍｏｌ／Ｌ,平均回收率为９７．５７±３．０４％,日内与日间的ＣＶ分别为３．２９％和５．０８％。     

溶剂萃取石墨炉原子吸收光谱测定盐卤中痕量铷

采用石墨炉原子吸收光谱（ＧＦＡＡＳ）研究盐卤中铷的原子化行为和机理,建立了热解石墨管,ＫＮＯ３－ＮＨ４ＮＯ３基体改进剂,１８－冠－６,溴百里香酚蓝,氯仿萃取分离ＧＦＡＡＳ测定盐卤铷的方法。用于测定盐卤中痕量铷,特征质量１．１×１０＾－１０ｇ／０．００４４,加标回收率８９％￣１１０％;相对标准偏差６．２８％（ｎ＝１３）。     

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.