微波辐射FeCl3催化无溶剂条件下的呐醇重排

通过微波辐射, 以FeCl3为催化剂进行无溶剂条件下的呐醇重排反应, 1 min产率可达86%～96%. 该方法具有操作简便、反应时间缩短、对环境友好等优点.     

Beckmann Rearrangement of Dimethylcyclopentanonepimarate Oxime

Beckmann rearrangement of dimethylcyclopentanonepimarate-15-oxime 2 was used to produce lactam 3 or seco-nitrile 4, depending on the conditions. The structures of the synthesized compounds were confirmed by IR and NMR spectroscopies.     

Beckmann重排法合成抗癫痫药加巴喷丁

由亚甲基环己烷出发, 采用[2＋2]环加成和Beckmann重排策略, 经四步反应在比较温和的条件下合成了抗癫痫药物加巴喷丁盐酸盐.     

A Novel Method for Beckmann Rearrangement of Oximes with Silica Sulfuric Acid under Mild Condition

The conversion of ketoxime into corresponding amide, known as the Beckmann rearrangement, is a common method used in organic chemistry and is also a topic of current interest. It accomplishes both the cleavage of carbon-carbon bond and the formation of a carbon-nitrogen bond, and represents a powerful method particularly for manufacture ε-caprolactam in chemical industry. This reaction, however, generally requires high reaction temperature, strong Br?nsted acid and dehydrating media, causing …     

Silica sulfate as a recyclable and efficient catalyst for Beckmann rearrangement under microwave irradiation

Silica sulfate has been proved to be an efficient and recyclable catalyst for Beckmann rearrangement of a variety of oximes in acetone under microwave irradiation. This protocol has advantages of high conversion, high selectivity, short reaction time, no environmental pollution, and simple work-up procedure.     

浅谈Beckmann重排反应在有机合成中的应用

本文讨论了Beckmann重排反应的机理以及酮肟的几何异构、催化剂的选择及溶剂对产物的收率和酰胺异构体比例的影响,并介绍了此重排反应在有机合成上的应用。     

Sulfuryl Fluoride Mediated Synthesis of Amides and Amidines from Ketoximes via Beckmann Rearrangement

A metal-free and redox-neutral method for Beckmann rearrangement employing inexpensive and readily available SO₂F₂ gas is described. The reported transformation proceeds at ambient temperature and is compatible with a wide range of sterically and electronically diverse aromatic, heteroaromatic, aliphatic and lignin-like oximes providing amides in good to excellent yields. The reaction proceeds through the formation of an imidoyl fluoride intermediate that can also be used for the synthesis of amidines.     

钴催化的高效贝克曼重排反应

利用廉价易得的氟硼酸钴水合物, 在温和、 无添加剂的空气条件下, 高效催化酮肟衍生物的贝克曼重排反应, 底物的普适性和官能团的兼容性均较理想, 产物收率最高达97%. 基于该高活性的氟硼酸钴水合物, 实现了10 g级二苯甲酮肟的贝克曼重排反应, 收率为71%. 同时, 也实现了钴催化酮类衍生物和盐酸羟胺的一步法贝克曼重排反应, 产物最高收率为94%, 反应体系中无溶剂及添加剂, 反应体系的原子经济性和底物普适性较好.     

微波干法催化环内酰胺N－烷基化反应

微波干法催化环内酰胺Ｎ－烷基化反应王存德，肖东运，张明，田兆斌，张霖（扬州大学工学院扬州２２５００１）关键词微波辐射，环内酰胺，Ｎ－烷基化，卤代烷Ｎ－烷基环内酰胺广泛应用于医药和日用化学品中［１，２］．近年来有关Ｎ－烷基环内酰胺的合成有：碱叔丁醇钾－...     

钛硅分子筛催化气相环己酮肟贝克曼重排反应

 对比研究了具有MFI结构的TS－1，silicalite－1，Al－ZSM－5和B－ZSM－5分子筛对气相环己酮肟贝克曼重排反应的催化性能．结果显示，TS－1适宜用作重排反应的催化剂，而含骨架B或Al的ZSM－5分子筛的催化性能较差，表明将Ti引入至sili－calite－1有利于改善其对环己酮肟重排反应的催化性能．反应氛围（溶剂、载气和原料添加物）对TS－1催化性能的影响规律说明，弱酸性气体的存在有利于TS－1对环己酮肟的活化与己内酰胺的选择性生成．优化的反应氛围包括以甲醇或乙醇为溶剂，二氧化碳为载气，以及醋酸为原料添加物．     

Carbon Tetrabromide/Triphenylphosphine‐Activated Beckmann Rearrangement of Ketoximes for Synthesis of Amides

An efficient Beckmann rearrangement of ketoximes was developed using carbon tetrabromide/triphenylphosphine as an organocatalyst without addition of any acids or metals. The reaction showed good functional group tolerance and gave various amides in moderate to good yields.     

微波辐射条件下季戊四醇双缩醛和双缩酮化合物的合成

微波辐射硫酸锆-硅胶催化季戊四醇与醛、酮缩合反应,高收率制得了双缩醛和双缩酮化合物.该方法操作简便,收率高,催化剂可重复使用,是一种环境友好型催化反应.     

Efficient Procedure for Beckmann Rearrangement of Ketoximes Catalyzed by Sulfamic Acid/Zinc Chloride

The Beckmann rearrangement of a variety of ketoximes to corresponding amides catalyzed by sulfamic acid and zinc chloride was carried out in good yields at refluxing temperature in acetonitrile.     

Condensation of Meldrum Acids with Carbonyl Compounds in Dry Media under Microwave Irradiation

以冰醋酸－六氢吡啶为催化剂，硅胶或氧化铝为载体，Ｍｅｌｄｒｕｍ酸与一系列醛酮在微波辐射下发生缩合反应，产率为２２～９７％。     

Microwave-Assisted Beckmann Rearrangement of Aryl Ketoximes Catalyzed by In(OTf)3 in Ionic Liquid

Abstract

Carbonyl compounds were regenerated from corresponding dithioacetals via refluxing with FeCl₃/KI and methanol as a solvent.     

微波辐射下2-芳基取代苯并噁唑的合成

邻氨基酚和芳香羧酸在微波辐射条件下缩合,合成了4种2-芳基取代苯并噁唑化合物。优化反应条件为：多聚磷酸为催化剂,辐射功率500W,辐射时间4min。     

微波干法催化醛酮与胺的缩合反应

利用微波辐射和固体中性Al2 O3 载体催化醛酮与胺的缩合反应的方法合成了十六种亚胺 ,研究了微波功率、作用时间、产物提取方式等因素对反应的影响 ;与无微波作用的一般合成方法相比 ,该法明显地提高反应速度及产率 ;文中用低极性熔点递变物质灌装毛细管的方法观测微波作用下反应温度 ,探讨微波作用化学反应的机理 ,其机理除与微波加热作用有关外还与分子间氢键及分子的缔合性有关。     

嘧啶酮衍生物的微波合成

在微波辅助下,Baylis-Hillman加成物与4-氨基-6-氯嘧啶或2-氨基-噻唑反应,快速合成了两类嘧啶酮衍生物——3-取代-7-氯-4H-嘧啶[1,2-b]哒嗪-4-酮和6-取代-5H-噻唑[3,2-a]嘧啶-5-酮,收率81%～98%,其结构经1H NMR,13C NMR,IR和MS确证。     

微波照射制备钛酸钡纳米晶

Cubic barium titanate nanocrystals were prepared by Ti(OC₄H₉)₄ and C₂H₅OH mixture with BaCl₂ aqueous solution under normal atmosphere microwave irradiation. Experiment results showed that when n_Ba / n_Ti=1.1, φ_EtOH=25%,highly dispersed barium titanate with particle size about 30 nm were completely formed by microwave irradiation only for 0.5 h. Microwave irradiation time had almost no effects on particle size and morphology of the product. Particle sizes were decreased with the increased EtOH amount, when φ_EtOH=50%, microwave irradiation 2 h, barium titanate nanocrystals with average size only about 22 nm were obtained.