微波辐射下吡啶[2,3-d]嘧啶衍生物的高效合成

本文以等摩尔的芳醛,巴比妥酸（或1,3-二甲基巴比妥酸）,5-氨基-2-甲基苯[d]噻唑为原料,以醋酸和乙二醇为溶剂,微波辐射下多组分一锅法合成了一系列新的吡啶[2,3-d]嘧啶衍生物。这种方法具有产率高,操作简便,反应时间短等优点。     

Crystal Structure of 4—（4—chlorophenyl）—7,7—dimethyl—2,5—dioxo—1,2,3,4,5,6,7,8—octahydroquinoline

1 INTRODUCTION Since the discovery of the pharmacological effects of 1,4-dihydropridines(1,4-DHPs) as calcium channel blocks[1], a great deal of work has been directed towards synthesis of the novel 1,4-DHPs acting as calcium antagonists[2, 3]. In fact, it is well-established that slightly modified structures on the DHP exhibit a calcium agents effect[4, 5] ; however, two fused rings have been less well-studied. By refluxing equivalent amounts of dimedone, aromatic aldehyde Meldrum抯 …     

Synthesis and Crystal Structure of 1-Phenyl-3-methyl-4-（4-bromophenyl）-6-（2-chlorophenyl）-pyrazolo[3,4-b] Pyridine under Microwave Irradiation

1INTRODUCTIONThepyrazolo[3,4-b]pyridineclassofcompoundspossessmanybiologicalandpharmacologicalactivi-ties[1],suchasactiveanti-concretionmedicaments[2]aswellasactiveanti-gramnegativeandpositivebacteriaagents[3].Thereforethesynthesesofsuchcompoundshavearousedgreatattentionofalargenumberofchemists.Themostimportantsyntheticrouteisthecondensationreaction[4～11]ofamino-pyrazoleandα,β-unsaturatedcompounds.Theorganicreactionundermicrowaveirradia-tionhastheadvantagesoffastreactionspeed,shorttime…     

Michael-Addition Reaction of Malononitrile with α,β-Unsaturated Cycloketones Catalyzed by KF／Al2O3

A series of KF/Al2O3 catalyzed Michael-addition reactions between malononitrile and α,β-unsaturated cycloketones in DMF solution were studied. At room temperature, 2-cyano-3-aryl-3-(1,2,3,4-tetrahydronaphthalen-1-one-2-yl) propionitrile derivatives were synthesized by the reaction between 2-arylmethylidene-1,2,3,4-tetra-hydronaphthalen-1-one and malononitrile. However, if the temperature was increased to 80℃, 2-amino-3-cyano-4-aryl-4H-benzo[h]chromene derivatives were obtained in high yields. When the α,β-unsaturated ketones were replaced by 2,6-biarylmethylidenecyclohexanone or 2,5-biarylmethylidenecyclopentanone, another series of 2-amino-3-cyano-4H-pyran derivatives was isolated successfully. The structures of the products were confirmed by X-ray diffraction analysis.     

“一锅法”合成11,11′-双(8,11-二氢苯并[f]呋喃并[3,4-b]喹啉-10-酮)(英文)

微波辐射下,不使用催化剂,在醋酸和DMF的混合溶剂中二醛、季酮酸和萘胺反应,"一锅法"合成11,11′-双(8,11-二氢苯并[f]呋喃并[3,4-b]喹啉-10-酮)。所合成化合物的结构经红外光谱、核磁共振光谱和高分辨率质谱予以确证。该方法具有产率高、操作简单、反应时间短等优点。     

在离子液体中一步法合成吡唑[5,4-b]-γ-吡喃衍生物

芳醛、丙二腈与4,5-二氢-3-甲基-5-氧代-1-苯基吡唑在离子液体[bmim][BF₄]中反应, 合成了2-氨基-4-芳基-3-氰基-5-甲基-7-苯基吡唑[5,4-b]-γ-吡喃衍生物, 该法快速、高效, 是一种洁净的合成方法. 产物的结构通过红外光谱、核磁共振氢谱和元素分析进行表征.     

无溶剂条件下合成2-[3-氧代-1,3-二(未)取代苯基丙基]-1,2,3,4-四氢萘-1-酮

以3,4-二氢-1-萘酮和查尔酮为原料,在K2CO3-NaOH存在下,无溶剂室温研磨反应,方便地得到2-[3-氧代-1,3-二(未)取代苯基丙基]-1,2,3,4-四氢萘-1-酮.该方法具有反应条件温和、操作简单和产率较高等优点,并通过IR,1HNMR,元素分析确定了产物的结构,3b晶体结构通过X衍射测定.     

一种新的六氢喹啉衍生物的NMR研究

应用¹H NMR,¹³C NMR,DEPT,¹H-¹H COSY,HSQC,HMBC等多种NMR实验测试分析方法,确证了一种新的六氢喹啉衍生物2,7,7-三甲基-4-(4-羟基-3-甲氧基）苯基-5-氧代-1,4,5,6,7,8-六氢喹啉-3-羧酸甲酯的结构,并对它的¹H、¹³C信号进行了归属.     

利用自由基引发的1,2-炔基迁移实现非活性烯烃的炔膦酰化

研究了1,4-烯炔衍生物与二芳基膦氧化物在银介导下发生的炔酰化反应.该反应利用自由基引发的1,2-炔基迁移策略合成了一系列γ-酮膦氧化物,产率适中.该反应机理可能涉及膦中心自由基与乙烯基的加成、3-exo-dig环化和1,2-炔基迁移等连续的过程,一步形成了C-P、C-C键等化学键,实现了非活性烯烃的双官能化.     

微波辐射下芳醛与5, 5-甲基-1, 3-环己二酮的固相和液 相反应

芳醛(1)与5,5-二甲基-1,3-环己二酮(2)在固相条件下,经微波辐射得到3,而在乙二醇溶剂中,经微波辐射得到4,产率接近定量。