脲醛树脂合成实验的改进

对中学教材中脲醛树脂制取实验中存在的结论性错误进行了澄清,对大学有机化学实验中脲醛树脂合成实验进行了合理的改进,并对实验过程中的注意事项包括原料配比、酸的选择、pH的确定、温度的选择进行了探索,最终所得工艺条件具有实验效果明显、容易操作及实用性强等诸多优点,适合新时期教改的需要。     

中学化学实验中的科学风险认知和决策意识

对中学化学实验中的科学风险认知和决策意识进行探索与思考,分析了中学化学实验中科学风险教育的现状,探讨了在化学实验中进行科学风险认知和决策的方式,阐述了在化学实验中培养学生科学风险认知和决策意识的意义。     

咖啡因的升华装置的优化和形象化展现

“茶叶中咖啡因的提取实验”是有机化学的一个经典实验。对传统的升华装置进行了改进,让升华实验更加简单高效,并且能够看到咖啡因晶体聚集和长大的过程,该装置便于咖啡因的收集,能对所收集的咖啡因进行定量计算,同时增加了采用薄层色谱法对浓缩液中咖啡因进行定性鉴定的实验环节。改进的实验丰富了实验内容,降低了实验可能的失误,提高了实验的安全性,创造性地运用实验室的显微熔点仪和智能手机成功地对咖啡因晶体的形貌进行了拍摄,增加了实验的趣味性。     

钠在氯气中燃烧实验的改进

指出了现行高中化学教材中钠在氯气中燃烧实验的不足,详细介绍了改进后的实验装置及其实验方法,简化了氯气制备及其实验过程,保障了整个实验在封闭体系内进行,解决了钠在氯气中燃烧实验严重污染环境问题,从而培养了学生的环保意识。     

探究性实验选题途径的实践研究

结合具体教学实践,介绍了探究性实验选题的6种途径,其中包括从教材知识中选题、从教材习题中选题、对教材中的原有实验方案进行创新探究、对实验仪器进行自制或改进、将疑难问题改为探究性实验及从现实生活中选题等,并提出了相应的思考。     

酯的水解实验的改进

该文对现行的高中化学 (试验修订本 )第二册中关于乙酸乙酯水解实验的不足之处进行了分析,并提出了改进的方法,对其实验内容和实验效果进行了讨论。     

电解水演示实验的探究

电解水实验为中学化学的一个经典演示实验,然而在实验中很难得到氢气和氧气的体积比为2∶1的结果。文章从离子电迁移率、超电势、溶液的酸碱度等影响电解水反应的主要因素入手,研究了电解水实验的科学原理,并运用这些原理结合改进后的实验装置进行了电解水实验过程的探究,获得了电解水实验的满意效果,很适合在课堂中进行演示。     

不可忽视的“化学实验教学设计”

化学实验在科学研究和化学学习中有着重要作用,化学实验教学设计意在教学理论的指导下,对实验的目标进行分解、实验内容进行改进与组合、实验过程进行优化、实验的效果进行评价。结合实施原则从3个方面对化学实验教学设计进行了探索。     

有机化学实验教学中合成实验反应进程的探讨

对现行有机化学实验教材中合成实验反应进程的监控和反应终点的判断问题进行了探讨,并以呋喃甲醇和呋喃甲酸的制备实验为例提出了对现行有机化学实验教材中合成实验的修改建议。     

含活泼质子水溶性化合物的核磁共振结构解析

利用核磁共振对在水溶剂易溶且含活泼质子的化合物的结构进行解析.实验中将待测样品直接溶解于二次去离子水中,并利用外标进行锁场.这样既保证了核磁共振实验的正常进行,同时避免了实验中氘代试剂对活泼质子的置换效应,为化合物中活泼质子的定位提供了直接的依据.为了保证外标锁场实验核磁共振谱图的质量,本工作采用了溶剂峰压制的核磁共振实验技术,获取了一组高质量的1D、2D谱图,并在此基础上顺利完成了对头孢米诺盐的结构确定.     

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.     

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.     

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 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.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

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.     

Microwave-assisted copper-catalyzed stereoselective ring expansion of three-membered heterocycles with α-diazo-β-dicarbonyl compounds

Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular S_N2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively.     

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.