新显色剂4—甲基—2—磺酸基苯基重氮氨基偶氮苯的合成及与镉的显色反？…

报道了新显色剂４－甲基－２－磺酸基苯基重氮氨基偶氮苯的合成及其与Ｃｄ（Ⅱ）的显色反应。实验表明,在非离子表面活性剂Ｔｒｉｔｏｎ Ｘ－１００存在下,于ｐＨ１０．８的氨水－氯化铵缓冲介质中,试剂与Ｃｄ（Ⅱ）形成３：１的红色络合物,最大吸收波长位于５２２ｎｍ处,Ｃｄ（Ⅱ）含量在０～２０μｇ／２５ｍＬ范围内符合比耳定律,表观摩尔吸光系数为２．０５×０５＾５Ｌ·ｍｏｌ＾－１·ｃｍ＾－１。已直接用于废水中微量     

重氮树脂的合成

重氮树脂的合成曹曙光赵超曹维孝＊（北京大学化学与分子工程学院北京１００８７１）关键词重氮树脂，合成，多聚甲醛１９９７－０２－０４收稿，１９９７－０７－１４修回国家自然科学基金资助课题二苯胺重氮盐与甲醛缩合生成的重氮树脂由于其感光速度快，亲墨性好，又易...     

（2E,4E）—3—苯基—2—（2—（N—乙氧羰基甲基氨基）—苯硫基）—2,4—己二烯酸乙酯

２，３－二氢－２－甲基－４－苯基－１，５－苯并硫氮杂卓与重氮乙酸乙酯反应，得到非预斯的分子内重排的开环产物，通过元素分析，ＩＲ，＾１ＨＮＭＲＭＳ及Ｘ－晶体的衍射分析确定了它的结构，并根据产物的结构，对这一新反应的反应机理进行了探讨和研究。     

双（N,N′—亚烃基—2,2′—（芳亚甲基）二（3,4—二甲基吡咯— …

首次报道了新型Ｓｃｈｉｆｆ碱类配体双（Ｎ，Ｎ′－亚烃基－２，２′－（苯亚甲基）－二（３，４－二甲吡咯－５－醛缩亚胺）和双（Ｎ，Ｎ′－（１，２－亚乙基）－２，２′－（４－甲氧基苯亚甲基）二（３，４－二甲基吡咯－５－醛缩亚胺）及其双锰配合物的合成方法，光谱特征及用配合物催化ＰｈＩＯ单加氧化环己环反应的研究。     

5－羟甲基－5－壬烷基戊内酯的合成

以已二酸为原料，经六步反应合成了５－羟甲基－５－壬烷基戊内酯，在形成手性中心的关键反应步骤中使用了（３Ｓ，４Ｓ）－１－苄基－１－甲基－３，４－二羟基吡咯碘化铵作手性相转移催化剂。     

铽与4—酰代吡唑啉酮—5的三元配合物的合成与荧光性质

合成并表征了一系列铽与含不同４－酰代的１－苯基－３－甲基－吡唑啉酮－５的三元配合物Ｔｂ９Ｌ）３．２Ｈ２Ｏ和Ｔｂ（Ｌ）３．Ｄｉｐｙ「Ｌ＝１－苯基－３－甲基－４－乙酰基吡啥林酮－５（ＰＭＡＰ），１－苯基－３－甲基－４－丙酰基吡唑啉酮－５（ＰＭＰＰ），１－苯基－３－甲基－４－异丁酰基吡唑啉酮－５（ＰＭＩＢＰ），１－苯基－３－甲基－４－特戊酰基吡唑啉酮－５（ＰＭＰＶＰ），１－苯基－３－甲基－４－苯甲酰基吡     

双[N,N‘—1,2—亚乙基—2,2’—（苯基亚甲基）二（3,4—二甲基吡？…

首次报道了一个新的拟酶模型物－双［Ｎ，Ｎ＇－１，２－亚乙基－２，２＇－（苯基亚甲基）二（３，４－二甲基吡咯－５－醋缩亚胺）］合双锰的合成方法及光谱特征；并对用ＰｈＩＯ单加氧化环己烷反应的催化性能及自氧化反应进行了研究。结果表明，此Ｓｃｈｉｆｆ碱双锰配合物的催化性能及稳定性与金属卟啉ＴＰＰＭｎＣｌ相似。     

反式—2—（4—（2—（4—取代苯基）乙烯基）苯基）—5—（4—联苯基）恶唑的合成,？…

通过４－ＲＣ６ＨＣＨＯ与２－（４－甲基苯基）－５－（４－联苯基）恶唑（Ｒ＝Ｈ，Ｍｅ，Ｅｔ，ｉ－Ｐｒ，ｉ－Ｂｕ，Ｐｈ，ＯＭｅ，Ｆ，Ｃｌ，Ｂｒ）在碱催化下的缩合反应合成了１０个新的反式－２－（２－（４－取代苯基）乙烯基）苯基）－５－（４－联苯基）恶唑类化合物，经元素分析，ＩＲ，ＵＶ及ＭＳ确定了它们的结构，并测定了荧光发射光谱，荧光量子产率和激光转换效率。     

希土与三甘醇—二(2, 2''—乙酰丙酮—4, 4''—甲基)苯基醚配合物的研究

以合成的一种新化合物三甘醇－二（２，２＇－乙酰丙酮－４，４＇－甲基）苯基醚作配体，在无水甲醇中合成了七种希土氯化物的配合物，确定其组成是ＬｎＬＣｌ（Ｌｎ：Ｌａ，Ｃｅ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ和Ｄｙ），Ｌ：三甘醇－二（２，２＇－乙酰丙酮－４，４＇－甲基）苯基醚。由ＩＲ，ＵＶ，ＴＧ－ＤＴＧ和display status     

聚（N—十二烷基—3—苯基吡咯）的研究

合成了一种吡咯的双取代衍生物：Ｎ－十二烷基－３－苯基吡咯，并用化学氧化法对其实施了聚合反应。该反应生成的导电聚合物可溶于一般有机溶剂，用溶剂蒸发制膜的方法可制得柔软的自支撑薄膜，用四电极方法测得掺杂态薄膜的电导率约为０．０５Ｓ／ｃｍ。并通过元素分析、ＧＰＣ、ＦＴ－ＩＲ、１Ｈ－ＮＭＲ等手段对其分子结构进行了表征。     

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.     

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.     

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.