“二氧化氮与水反应”的实验探究

在探究教学中,我们自制了“二氧化氮与水反应”微型实验装置,并引导学生对NO2的制取、收集、NO2与水反应的定性和定量等方面进行实验探究和理论分析,使学生体验化学研究过程,激发学习化学的兴趣,较好地探索和验证了氮化物存在的多种形态和反应体系的复杂性。     

绿色简易法制备纯二氧化氮气体

设计了一种在密闭容器中制备纯二氧化氮气体的绿色简易方法。该方法实现了气体制备、收集、尾气处理的一体化，不仅可用于课堂演示实验，也为深入研究二氧化氮溶于水的定量实验奠定物质基础。另外，此方法也可用于无氧环境下其他物质的制备。     

二氧化氮的“喷泉实验”

氨(或氯化氢)极易溶于水的喷泉实验,中学化学课本已作了介绍;利用二氧化氮气体与水反应生成硝酸的“喷泉实验”,则尚未见报道。本文将介绍这一演示实验。     

氨氧化制硝酸演示实验

氨氧化制硝酸的演示实验,对学生掌握氨氧化制硝酸的工业生产原理及观察催化剂的催化现象有良好作用。几年来,在多次演示实验中,我们对催化剂的选择、氨气浓度的控制以及实验装置等问题进行了一些摸索和改进,通过本演示实验,能使学生观察到氨氧化放热使催化剂烧红,生成的一氧化氮被氧化为红棕色的二氧化氮,二氧化氮被水吸收生成硝酸等非常鲜明的现象。     

“热平衡安瓿”演示器的制作与使用

温度对化学平衡影响的演示实验和学生实验使用的是二氧化氮,在二氧化氮的制取和实验过程中都会有一定的二氧化氮泄漏到空气中,污染空气,毒害人体。为此我们特作如下改进。     

二氧化氮溶于水的定量实验

本实验说明以下四点:1.二氧化氮溶于水生成硝酸,并生成1/3体积的无色一氧化氮气体。2.生成的硝酸具有酸性。     

氮元素正价变化组合实验探究

将二氧化氮的制备、二氧化氮溶于氢氧化钠溶液形成喷泉、一氧化氮被氧气氧化为二氧化氮等实验进行巧妙的整合,可实现含氮化合物中氮元素正化合价循环变化：HO3O2HO2O,由此形成固定的实验装置和较好的实验方案,可用于含氮化合物知识与预防其污染的探究教学。     

探究二氧化氮气体的助燃性

针对教学中学生提出的有关二氧化氮气体助燃性的问题,以实验为手段进行了相关探究,考察了部分可燃物在二氧化氮气体中的燃烧情况,并分析了NO2具有助燃性的原理以及助燃特点。     

浓硫酸不能干燥NO2的实验探究

二氧化氮为红棕色、有强烈刺激性气味、有毒性的气体.易溶于水,且能与水反应的一种酸性氧化物.在实验室制取NO2时,能否用浓H2SO4来干燥NO2气体,一般化学参考资料都没有明确指出,大学教材[1]中的有关内容也是如此.但是目前在一些权威性著作[2]中出现"浓硫酸可以用来干燥NO2气体".在一些高中化学复习资料中,用浓硫酸来干燥NO2的练习和测试题频频出现.然而,这是一个十分明显的科学性错误.下面笔者就先用2个实验的客观现象来说明浓硫酸不能用于干燥二氧化氮气体.     

氯水性质检验的微型实验设计

采用以双通管为主体的复合微型实验装置,4 min 内完成了氯水的制备、氯水颜色的观察、氯水的萃取、氯气与水反应产物H+与Cl-的检验、氯水漂白性的实验。     

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.     

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.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

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.