Solid‐Supported Green Synthesis of Substituted Hydrocinnamic Esters by Focused Microwave Irradiation

An efficient chemoselective hydrogenation protocol for substituted cinnamic esters is developed for the synthesis in quantitative yield of corresponding bioactive dihydrocinnamic esters with solid‐supported palladium chloride/ammonium formate (cat.) in HCOOH/H₂O 1 : 2 as a hydrogenating agent under focused‐microwave irradiation for 10 min.     

Synthesis of Substituted Salicylanilides under Microwave Irradiation

Summary. Salicylanilides were prepared in 70–95% yields in 4–8min from phenyl salicylate or phenyl 4-methoxysalicylate and substituted anilines under microwave irradiation under solvent free conditions.Received October 17, 2002; accepted October 22, 2002 Published online July 3, 2003     

Solid Supported Synthesis of New 2,4‐Dithioxo‐6‐aryl‐3‐(1′,3′,4′‐thiadiazolo)‐1,3,5‐triazines Using Microwaves

A series of novel 2,4‐dithioxo‐6‐aryl‐3‐(1′,3′,4′‐thiadiazolo)‐1,3,5‐triazines have been synthesized from 1,3,4‐thiadiazolo‐thioureas and arylaldehydes using microwave irradiations (MWI) over inorganic solid supports. The yield afforded in microwave reactions was 80% whereas it was 60% in conventional reactions. Solid supported synthesis using microwaves has eliminated the usage of toxic substances and organic solvents except for the limited consumption of methanol and ethanol in pre and post reaction stages. This methodology has been proved an efficient, facile, rapid, and ecofriendly synthetic technology.     

Unexpected One‐pot Synthesis of Novel 2‐Aminopyrimidine‐4‐ones under Microwave Irradiation

One‐pot, three‐component condensation of guanidine, ethylbenzoylacetate and various aromatic aldehydes in the presence of NaHCO₃ have been investigated by microwave irradiation. The aromatic aldehydes bearing electron‐withdrawing groups undergo condensation with guanidine and ethylbenzoyl‐acetate to afford ethyl‐2‐amino‐4‐aryl‐1,4‐dihydro‐6‐phenylpyrimidine‐5‐carboxylate derivatives via Biginelli reaction. However, reaction of the aromatic aldehydes having electron‐releasing groups with guanidine and ethylbenzoylacetate did not give the corresponding dihydropyrimidines. Instead, novel 2‐amino‐5‐benzoyl‐5,6‐dihydro‐6‐arylpyrimidine‐4(3H)‐ones were obtained via an unexpected mechanism.     

I2‐Catalyzed Divergent Regioselective Addition of Methoxybenzenes with Ethenylbenzenes under Microwave Irradiation

A highly efficient synthesis of 1,2,2‐triarylethanones has been developed from simple and commercially available electron‐rich arenes and styrenes (ethenylbenzenes).     

Solid State Desemicarbazonation on Clayfen Under Microwave Irradiation

Summary.  A new, efficient, and environmentally benign method for the cleavage of semicarbazones has been achieved by a simple reaction of semicarbazones with clayfen under microwave irradiation. Received January 4, 2001. Accepted (revised) March 1, 2001     

微波辐射下固相反应合成二苯基甲基醚

在常压下用微波辐射固相反应的方法合成了二苯基甲基醚,与用有机溶剂为介质及传统的热固相反应方法相比,其反应速率快,产率高。     

微波辐射固体酸催化合成马来酸双酯

首次在微波辐射下，用活性炭固载对甲苯磺酸催化合成了马来酸双酯．当微波辐射功率为150W．正辛醇：酸酐＝3：1，催化剂用量为2．5g时，反应20min后，马来酸酐转化率达89．8％，产物的选择性为99．5％．同时，也发现随着醇的炭数增多，反应温度和反应速率增加；在微波辐射条件下，酯化反应速率、产物选择性都高于常规加热方式下的反应结果．     

微波辅助固相有机反应

固相有机合成是组合化学中构建化合物库的主要工具之一［１,２］,但是,由于它是连接在固相载体（如树脂等）上的试剂与溶解在有机溶剂中的试剂之间的反应,因此反应比较缓慢．考虑到微波技术对有机反应的协助作用,我们将微波技术应用到固相有机反应中,对比研究了微波...     

Zeolite‐Supported One‐Pot Synthesis of Bis‐azetidinones under Microwave Irradiation

In an attempt to synthesize antibacterial agents effective against gram‐positive and gram‐negative bacteria, the efficient synthesis of novel bis‐azetidinones ( 3a–j ) has been established. Thus, cycloaddition reaction of substituted bis‐imines with chloroacetylchloride under microwave irradiation in the presence of zeolite yielded bis‐azetidinones ( 3a–j ). Structures of the synthesized compounds have been elucidated on the basis of their elemental analysis and spectral data (IR, ¹H‐NMR, ¹³C‐NMR, and mass spectra). The synthesized bis‐azetidinones were screened for their antibacterial activity against five microorganisms: Bacillus subtilis, Proteus vulgaris, Staphylococcus aureus, Klebsiella pneumoniae, and Escherichia coli. They were found to exhibit good to moderate antibacterial activity.     

Cycloaddition Reaction of Epoxides with Various Alkenes Under Microwave Irradiation

Abstract

The reactivity of gem-dicyano epoxides with various alkenes is studies in solvent free conditions, and in homogeneous solution, under microwave irradiation. Microwave heating of these substrates in solvent, yields carbonyl ylides which give 1-3-dipolar cycloaddition.     

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。     

Microwave Activated Solid Support Synthesis of New Antibacterial Quinolones

Summary.  A novel synthesis of 6-fluoro-7-(5-aryl-1,3,4-thiadiazol/oxadiazol-2-yl-sulfanyl)-4-quinolone-3-carboxylic acids from 7-chloro-6-fluoro-4-quinolone-3-carboxylic acid and 5-substituted 1,3,4-thiadiazoles/oxadiazoles on basic alumina under microwave activation is described. All compounds were screened for their in vitro antibacterial activity against B. lichenformis, 2689, K. aerogens 2281, S. typhimurium 2501, E. herbicola 2491, and P. vulgaris 2027 and found to possess activities comparable to that of the standard drug norfloxacin. Received May 2, 2000. Accepted (revised) June 13, 2000     

微波辐射下4,6-二羟基嘧啶与醛的反应研究

以甲胺为催化剂、醋酸为溶剂, 微波促进下芳香醛与两分子4,6-二羟基嘧啶反应得到6-羟基-5-[(4-羟基-6-氧代-1,6-二氢嘧啶-5-基)芳甲基]嘧啶-4(3H)-酮衍生物.     

A Simple,Mild and Efficient One‐Pot Synthesis of 2‐Substituted Benzimidazoles in the Presence of H2O2/HCl under Microwave Irradiation

A simple, fast and efficient method for the preparation of several 2‐substituted benzimidazole derivatives is reported. Compounds were synthesized through a rapid one‐pot synthesis via microwave irradiation, starting from aldehydes and o‐phenylenediamine, in the presence of H₂O₂/HCl system in acetonitrile. The significant features of this method are short reaction times, high yields, easy and quick isolation of the products.     

Microwave assisted syntheses of 2,5-disubstituted 1,3,4-oxadiazoles

2,5-Disubstituted 1,3,4-oxadiazoles have been synthesized by oxidation of 1-aroyl-2-arylidene hydrazines with potassium permanganate on the surface of a solid mineral support as well as in mixtures of acetone and water under microwave irradiation.     

Environmentally Sustainable and Chemo‐selectively Favorable Synthesis of Substituted 2H‐Pyran‐2‐ones in Water under MWI

In this paper, a novel synthesis of diversely substituted 2H‐pyran‐2‐ones via the tandem reaction of 3‐hydroxyhexa‐4,5‐allenic esters in water under the promotion of MWI has been developed. Compared with those reactions carried out in organic solvents, water mediated synthesis of poly‐substituted 2H‐pyran‐2‐ones is not only environmentally sustainable, but also chemo‐selectively favorable.     

Study of SNAr Reactions of Halobenzenes with Imidazole under Ultrasonic and Microwave Irradiation

Summary. Nucleophilic aromatic substitution reactions with imidazole of haloarenes having strongly electron-withdrawing groups were studied under ultrasonic and microwave irradiations. The course of the S_NAr reactions was found to be strongly dependent on the electron-withdrawing properties of the substituents as well as on the leaving ability of the halogen atom. Microwave irradiation allowed to shorten the reaction time and to increase the yields compared with ultrasonic irradiation.     

Rapid Synthesis of 1,2,3,4-Tetrahydropyrimidin-2-ones Using Zn（NH2SO3）2 as a Catalyst under Microwave Irradiation

Rapid synthesis of 1,2,3,4-tetrahydropyrimidin-2-ones （THPO） from aromatic aldehydes, β-ketoester and urea （or thiourea） using zinc sulfamate as the catalyst under microwave irradiation was described here. Compared with the classical Biginelli reaction, this new method consistently has the advantages of good yields （76%-96%）, short reaction time （3-15 min）, no corrosion to equipments, ease of manipulation, and low cost catalyst.