硝酸铁催化氧化二芳基乙醇酮制备二芳基乙二酮

用AcOH作溶剂,PEG400做相转移催化剂,硝酸铁能将二芳基乙醇酮催化氧化为二芳基乙二酮。产物结构用IR,MS和1H NMR光谱对其进行了表征。该方法有反应时间短,产率较高,操作简便等优点,是一种有效的由二芳基乙醇酮氧化制备二芳基乙二酮的方法。     

微波辐射下蒙脱土K10固载氯化铁氧化二芳基乙醇酮

微波辐射下以蒙脱土K-10固载氯化铁为氧化剂, 氧化二芳基乙醇酮生成二芳基乙二酮化合物, 反应时间短, 产率高, 操作简便, 污染小, 是一种有效的由二芳基乙醇酮氧化制备二芳基乙二酮的方法.     

固体酸催化合成二芳基甲酮化合物的研究进展

二芳基甲酮化合物是一类非常重要的化工产品和医药中间体,广泛应用于医药、涂料、电子及日用化工等领域综述了在不同类型固体酸催化下,利用Friedel-Crafts酰基化反应合成二芳基甲酮化合物的研究进展.     

1,5-二芳基二酮衍生物的制备一无溶剂状态下苯乙酮与芳基烯酮的共轭加成反应研究

使苯乙酮作为亲核体,在无溶剂条件下,利用碱催化与烯酮发生共轭反应,合成了一系列新的1,5-二芳基二酮化合物.反应温和而方便、快速,收率在71～90%.     

超声条件下芳基格氏试剂与4-烷基苯乙酮的反应

二芳基乙烯;超声条件下芳基格氏试剂与4-烷基苯乙酮的反应     

3,4-二芳基吡咯酮衍生物的合成和生物活性

考布他汀-A4(Combretastatins-A4,CA-4)是从天然产物中分离得到的抗癌活性化合物,其分子中Z-构型烯键易异构化转变为无抗癌活性的E-构型.以吡咯-2,5-二酮或吡咯-2-酮代替烯键,设计合成了4个新的CA-4类似物.它们的合成是以3,4-二甲氧基苯乙酮或3-氟-4-甲氧基苯乙酮为起始原料,经α-溴化、改良的Gabriel合成法、与3,4,5-三甲氧基苯乙酸缩合、环化-氧化或环化四步反应完成.其结构用1H NMR,13C NMR,ESI-MS及元素分析进行了表征.用MTT法测试了CA-4类似物对人白血病细胞HL-60、肝癌细胞SMMC-7721和肺腺癌细胞A549的体外抗肿瘤活性.初步结果表明,含氟化合物3,4-二芳基-2,5-吡咯酮(1b)的抗肿瘤活性接近CA-4,IC50值达到0.03～0.05μmol·L-1.     

负载FeCl~3的皂土催化合成二芳基酮

在负载FeCl~3的皂土上由苯甲酰氯和苯甲醚发生Friedel-Crafts酰化反应合成了系列二芳基酮化合物,该方法具有产率高,操作简单,催化剂易再生等优点。     

1-烷基-4,6-二芳基四氢三嗪硫酮化合物的合成及其氧化反应

三芳基缩二胺与烷基硫脲在二氧六环回流条件下反应, 可生成1-烷基-4,6-二芳基四氢三嗪硫酮化合物3。利用芳香醛, 烷基硫脲和醋酸铵一锅法也能得到3, 而三芳基缩二胺与芳基硫脲反应, 则生成了咪唑啉的硫氰酸盐。室温下,在相转移催化剂TEBA存在时, 3可被高锰酸钾氧化, 得到1-烷基-4,6-二芳基-2(1H)三嗪酮化合物。     

醋酸溶液中2,3-二芳基-喹喔啉的简便合成

1,2-二芳基乙二酮与1,2-苯二胺在室温醋酸溶液中反应数分钟,生成2,3-二芳基一喹喔啉.反应时间短(1～10min),产率高(90%～97%),反应条件温和,操作简便.     

芳基硼酸对醛酮的加成反应的研究进展

芳基硼酸与醛酮的加成反应在最近几年受到了广泛的关注,综述了十多年来各种过渡金属催化的芳基硼酸对醛酮的加成反应的发展概况.     

Methyltrioxorhenium catalyzed oxidation of 1,2-diols to 1,2-diketones using hydrogen peroxide as oxidant

A variety of 1,2-diols were oxidized selectively to the corresponding 1,2-diketones by the dropwise addition of 30% aqueous hydrogen peroxide using methyltrioxorhenium as catalyst.     

Heterogeneous platinum catalytic aerobic oxidation of cyclopentane-1,2-diols to cyclopentane-1,2-diones

A method for the aerobic oxidation of cyclopentane-1,2-diols to the corresponding diketones over a commercial heterogeneous Pt/C catalyst is described. Unsubstituted and 3- or 4-substituted cyclopentane-1,2-diols are oxidized to 1,2-dicarbonyl compounds in good yields under the reported optimized reaction conditions (atmospheric air, 1 mol % of catalyst, 1 equiv of LiOH, aqueous solvents and 60 °C temperature). The method is applicable for producing cyclopentane-1,2-diketones in a scalable manner.     

Straightforward Synthesis of 1,2-Amino Phosphate Diesters and Application to the Synthesis of Novel 1,2-Amino Ether Diesters

A variety of 1,2-amino alcohol diesters 1 reacted smoothly with diethyl chlorophosphate under basic conditions to afford the corresponding 1,2-amino phosphate diesters 2 in excellent yields. These compounds served as useful precursors for subsequent nucleophilic attack by alcohols in an S_N2 fashion to provide 1,2-amino ether diesters 3.     

Sonogashira cross-coupling of 3-bromo-1,2-diones: an access to 3-alkynyl-1,2-diones

A new general method for the synthesis of enols of cyclic 3-alkynyl-substituted 1,2-diketones is developed. Sonogashira cross-coupling of silyl enolates of cyclic 3-bromo-cyclopentane- and 3-bromo-cyclohexane-1,2-diones with variety of substituted acetylenes afforded enols of cyclic 3-alkynyl-1,2-diones with good yields (up to 93%) in a short reaction time. The starting 3-bromo-1,2-diones are easily obtainable by direct bromination of 1,2-diones with NBS.     

Electrochemical study of 1,2-Naphthoquinone-4-sulphonate and 1,2-Naphthoquinone semicarbazone

Summary A study of the electrochemical characteristics of 1,2-naphthoquinone-4-sulphonate, sodium salt, and of the semicarbazone of 1,2-naphthoquinone (Naftazone) was carried out using d.c., a.c. and d.p. polarography and cyclic voltammetry. Changes in the waves as a function of concentration and pH indicate evidence of adsorption phenomena at the potential of the reduction wave. These techniques also indicate the formation of a mercury derivative in the case of Naftazone. The quantitative determination of these two compounds is possible by polarography. Limits of detection are 5×10^–6 and 5×10^–8 M, respectively.

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Elektrochemische Untersuchung von 1,2-Naphthochinon-4-sulfonat und 1,2-Naphthochinon-semicarbazon

Zusammenfassung Die elektrochemischen Eigenschaften von 1,2-Naphthochinon-4-sulfonat und -semicarbazon (Naftazon) wurden mit Hilfe der Gleichstrom-, Wechselstrom und Differentialpuls-Polarographie sowie der cyclischen Voltammetrie untersucht. Veränderungen an den Stufen in Abhängigkeit von Konzentration und pH-Wert deuten auf Adsorptionsvorgänge beim Potential der Reduktionsstufe hin. Im Falle von Naftazon wurde die Bildung eines Quecksilberderivats nachgewiesen. Beide Substanzen können polarographisch mit Nachweisgrenzen von 5×10^–6 bzw. 5 × 10^–8 M bestimmt werden.

     

Facile Preparation of 1,2-Diketones

Easily accessible lead-like libraries of heterocyclic molecules useful for high-throughput screening are of continuous interest to the pharmaceutical industry. A number of drug-like libraries are derived from aromatic 1,2-diketones; however, nonsymmetrical 1,2-diketones are challenging to prepare. This communication describes a simple and practical synthesis of 1,2-diketones based on a controlled cross benzoin-like condensation reaction.     

Novel 3-Cyanosubstituted 1,2-Thiaphosphacyclanes: Synthesis and Stereochemistry

The facile synthetic route to 5- and 6-membered 3-cyano-2-oxo-1,2-thiaphosphacyclanes and 6-cyano-2-oxa-10-oxa(thia)-phosphabicyclo [4.4.0]-decane-1-oxides was elaborated via intramolecular S-alkylation in a series of y -haloalkylsubstituted thiophosphorylacetonitriles. The compounds were used to prepare novel P(III)-containing bidentate ligands with definite stereochemistry. Diastereomeric transformations among 2-oxo-1,2-thiaphosphinanes were found and the mechanism of such transformations is suggested.     

Synthesis of 1,2-bis(methoxyamino)cycloalkanes from alicyclic 1,2-bis(hydroxyamines)

Derivatives of 1,4-dihydroxypiperazine-2,3-dione were obtained by reaction of cis-1,2-bis(hydroxyamino)cycloalkanes with diethyl oxalate. Their alkylation with CH₂N₂ or Mel afforded 1,4-dimethoxypiperazine-2,3-diones. Hydrolysis of the latter gave 1,2-bis(methoxyamino)cycloalkanes.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 925–929, April, 1996.