磁性阳离子交换树脂的结构与性能分析

利用古埃磁天平法、扫描电镜、粉末Ｘ射线衍射以及分光光度法等检测了化学转化法制备的磁性阳离子交换树脂。结果表明,所制备的树脂内部磁性物质为Ｆｅ３Ｏ４,且在 树脂内部的孔道及表面分布均匀,均被封锁在树脂内部,因而,这类磁性树脂在碱性和中性盐溶液中具有较高的稳定性。此外,树脂的磁化过程并不影响其交换容量。     

球形纤维素基磁性阳离子的化学转化制备及机理研究

通过正交设计实验确定了用化学转化法制备球形纤维素基磁性阳离子交换树脂的最佳条件,即:将树脂在室温下浸渍于摩尔比为1∶2的Fe3 与Fe2 混合铁盐溶液中90min,然后,加入2mol/L的NaOH溶液,在搅拌下转化20min,Fe3 、Fe2 将转化为FeFe2O4并将均匀的分布在树脂的表面及大孔结构中,从而获取磁性树脂.并初步探讨了阳离子交换树脂磁化的机理.     

离子交换树脂用作聚合物试剂方面的新进展

本文综述由离子交换树脂为原料制备的聚合物离子型试剂.绝大多数的聚合物离子型试剂是用强碱性阴离子交换树脂制备的,它包括氧化剂、还原剂、20余种亲核试剂以及卤化剂等.约有40多种聚合物试剂可全由强碱性阴离子交换树脂制备.由强酸性阳离子交换树脂所制成的试剂只有数种.弱酸性阳离子交换树脂所制成的试剂,只是刚刚开始.弱碱性阴离子交换树脂可制成的试剂几乎没有.     

732^#强酸性阳离子交换树脂催化缩醛和缩酮的合成

本文研究了732＃强酸性阳离子交换树脂对缩醛和缩酮的催化作用，系统地探讨了各反应因素对反应的影响，研究发现，732＃强酸性阳离子交换树脂具有较高的催化活性，并使后处理简化。     

离子交换法提取谷氨酸的研究(Ⅰ)

本文分析了等电点—离子交换法提取谷氨酸的工艺特点,研究了弱酸性阳离子树脂优先脱铵的可行性和操作条件,提出了“弱酸性树脂脱铵—等电点结晶—强酸性树脂吸附谷氨酸”的工艺流程,并将其效果与文献资料进行了比较。     

球形纤维素磁性阴离子交换树脂的化学转化制备及特性研究

自制了大孔球形纤维素基阴离子交换树脂(PSC-AN),并利用化学转化法成功制备了大孔球形纤维素基磁性阴离子交换树脂(PSC-MAN)。对影响树脂质量磁化率的几个主要因素进行了探讨,实验确定最佳制备条件为:铁盐的配比为1∶10,EDTA的浓度为0.005 mol/L。对树脂的结构和性能进行了研究,表明化学转化法制备大孔球形纤维素基阴离子交换树脂(PSC-MAN)磁性强,在碱液中相当稳定,树脂磁化前后交换容量分别为Q前=1.33 meq/g、Q后=1.16 meq/g,即树脂基的交换容量基本不受磁化过程的影响。     

强酸性阳离子交换树脂催化合成马来酸二异戊酯

以强酸性阳离子交换树脂为催化剂催化异戊醇与马来酸酐反应合成了马来酸二异戊酯。在马来酸酐50mmol，异戊醇200mmol和强酸性阳离子交换树脂4.0g，回流分水60min的条件下，马来酸二异戊酯收率达92.2%，树脂重复使用5次，其活性未发生明显的变化。     

用阳离子交换树脂和pH梯度洗脱分离头孢菌素混合物

合成了一种聚苯乙烯结构的凝胶型1×2强酸性阳离子交换树脂,结合pH梯度或盐浓度梯度洗脱法分离头孢菌素类抗生素的混合物,并与市售的树脂比较,考察其分离性能。1×2型树脂具有较小的颗粒度(0.2～0.3mm)和较小的交换容量(在60%乙醇溶液中),用pH梯度洗脱法可以将5种头孢菌素按照等电点顺序完全分离,结构稳定的3种头孢菌素的收率均大于95%,1×2型强酸性阳离子交换树脂结合pH梯度洗脱法适用于水溶性头孢菌素类抗生素的制备分离。     

合成乳酸正丁酯的主要催化剂述评

综述聚氯乙烯—三氯化铁树脂、强酸性阳离子交换树脂、氨基磺酸、甲基磺酸、维生素C、稀土化合物、硅胶固载硫酸钛、硫酸铁铵、硫酸氢钠、磁性固体超强酸、酸改性高岭土、杂多酸(盐)等数种不同催化剂催化合成乳酸正丁酯的实验结果.结果表明,强酸型阳离子交换树脂、硫酸氢钠、磁性固体超强酸、硅胶固载硫酸钛、活性炭固载杂多酸五种催化剂催化合成乳酸正丁酯的酯收率较高,具有实际使用价值.     

离子交换法提高L-赖氨酸回收率的一些研究

我们研究了某些阳离子交换树脂对L-赖氨酸吸附容量与实验条件如溶液的pH值、浓度和流量之间的关系,探索了应用铵式强酸性阳离子交换树脂提高L-赖氨酸回收率的某些途径。     

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.