微波作用下亚烃基丙二酸亚异丙酯的合成

报导了微波辐射下丙二酸亚异丙酯与羧基化合物进行了Ｋｎｏｅｖｅｎａｇｅｌ缩合反应，高产率地合成了亚烃基丙二酸亚异丙酯。     

亚烃基丙二酸亚异丙酯的共轭加成-α -烃化串联反应

亚烃基丙二酸亚异丙酯与格氏试剂的共轭加成和α-烃化串联反应提供了一种合成不对称双取代丙二酸亚异丙酯的新方法。由于不对称双取代丙二酸亚异丙酯易水解失羧和醇解失羧转化成相应的羧酸及酯,因此本法也是合成α-及β-高取代的羧酸及其酯的有效方法。     

苯基(苯乙炔基)对甲苯磺酸碘(Ⅲ)的应用──5-烃基-5-苯乙炔基丙二酸亚异丙酯的合成

近年来，随着元素周期表中第VA，VIA族元素有机化合物在合成中得到了广泛的应用，激起人们对有机高价碘化物在合成中应用的兴趣［’－‘j．苯基（快基）碘盐（1）是具有多个亲电中心的化合物，在不同亲核试剂的作用下，分子中有3个部位可受到进攻［‘”j．由于通常的炔基卤化物对许多条核试剂的反应比较惰性，或者产物较为复杂，在合成上的应用受到限制．而化合物1作为快基的阳离子等效体的反应在会成上则很有价值＊，。‘．5一烃基丙二酸亚异丙酯在有机合成中是具有多种反应性能的试剂，同时又是许多热解反应的有效前体．至今，有关5一取…     

5-单取代丙二酸亚异丙酯的简便合成法

5-单烃基取代的丙二酸亚异丙酯是重要的有机合成中间体^[1],由于它的活性亚甲基具有较强的酸性(pK_a=4.75),用卤代烃直接烃化时,往往生成5,5-双取代产物^[2,3],所以一般用间接方法合成5-单取代丙二酸亚异丙酯^[4～6],其中以丙二酸亚异丙酯与羰基化合物缩合成亚烃基丙二酸亚异丙酯,继而还原的两步法最为普遍,常用的还原方法和还原剂有催化氢化、氢化铝锂,硼氢化钠等^[6]。     

合成丙二酸亚异丙酯Mannich碱的新方法

以甲醛和胺作为胺甲基化试剂，合成了丙二酸亚异丙酯及其5－单取代烃基衍 生物的Mannich碱，同时还讨论了这些Mannich碱的化学性质。     

5-烃基丙二酸亚异丙酯的Mannich碱与甲基酮的缩合反应

5-烃基丙二酸亚异丙酯的Mannich碱和甲基酮在弱酸如醋酸的存在下, 合成得到缩合产物5-(3-氧代烃基)丙二酸亚异丙酯(3).     

邻苯二甲酸异丙酯酰氧基-丙烯酰氧基-乙酰乙酸乙酯络铝及其聚合物的合成与荧光性质

通过异丙氧基铝和邻苯二甲酸酐、乙酰乙酸乙酯及丙烯酸反应,合成了螯合物单体邻苯二甲酸异丙酯酰氧基-丙烯酰氧基-乙酰乙酸乙酯络铝,由自由基聚合法合成了聚合物,用元素分析仪、VPO、IR、¹HNMR和²⁷AlNMR证实了它们的结构,并研究了它们在DMF中的荧光性质。     

超声波作用下芳亚甲基丙二酸亚异丙酯的合成

在超声波辐射下，以芳香醛、丙二酸亚异丙酯为原料，乙醇作溶剂，无催化剂 作用下合成了芳亚甲基丙二酸亚异丙酯。该方法操作简便，不污染环境，产率较高 ，为该类化合的合成提供了一种有效的新方法。     

二(顺丁烯二酸异丙酯酰氧基)-异丙氧基钕及其与甲基丙烯酸甲酯共聚物的研究

用三异丙氧基钕与顺丁烯二酸酐反应合成含钕单体二（顺丁烯二酸异丙酯酰氧基） 异丙氧基钕，并与甲基丙烯酸甲酯（ＭＭＡ）共聚而制得含钕共聚物．用元素分析、ＩＲ、ＸＰＳ和ＳＥＭ对其结构进行表征，并研究了其热性能、光学性能和磁性．表明含钕共聚物是一种具有优异热稳定性、高透光率和大折光率，以及具有光选择吸收性和顺磁性的高分子材料     

One‐Pot Synthesis of α‐Formyloxy Ketones from Enolizable Ketones

One‐pot synthesis of α‐formyloxy tones as well as α‐acetoxy ketones from enolizable ketones and [hydroxy(tosyloxy) iodo] benzene (HTIB)/polymer supported [hydroxy(tosyloxy) iodo] benzene (PSHTIB) in N,N–dimethylformamide (DMF)/N, N–dimethylacetamide (DMA) in high yields is described.     

Selective Oxidation of Sulfides to Sulfoxides With Poly[4‐Hydroxy(tosyloxy)iodo]styrene

Sulfides can be selectively converted to corresponding sulfoxides in excellent yields under mild conditions by linear and 1% cross‐linked poly[4‐hydroxy(tosyloxy)iodo]styrene (PSHTIB).     

Facile One‐Step Conversion of Ketones into α‐Azidoketones using [Hydroxy(tosyloxy)iodo]benzene and Sodium Azide in the Presence of a Phase‐Transfer Catalyst under Solvent‐Free Conditions

We have described a one‐step, solvent‐free synthesis of α‐azidoketones from the corresponding ketones that requires relatively benign [hydroxy(tosyloxy) iodo]‐benzene reagent, sodium azide, and phase‐transfer catalyst at room temperature. Generality of the protocol has been demonstrated by synthesizing various α‐azidoketones high in yield and purity within a short time.     

Hypervalent Iodine in the Synthesis of Bridgehead Heterocycles: A Facile Route to the Synthesis of 6‐Arylimidazo[2,1‐b]thiazoles Using [Hydroxy(tosyloxy)iodo]benzene

α‐Tosyloxyketones (2), readily accessible through hypervalent iodine oxidation of enolizable ketones (1) using [hydroxy(tosyloxy)iodo]benzene (HTIB) in acetonitrile, exclusively generates the 6‐arylimidazo[2,1‐b]thiazoles (4) on treatment with commercially available 2‐aminothiazole (3).     

A facile one-pot synthesis of β-keto sulfones from ketones under solvent-free conditions

An easy solvent-free method is described for the conversion of ketones into β-keto sulfones in high yields that involves the in situ generation of α-tosyloxyketones, followed by nucleophilic substitution with sodium arene sulfinate in the presence of tetra-butylammonium bromide at room temperature. The salient features of this one-pot protocol are short reaction times, cleaner reaction profiles, and simple work-up that precludes the use of toxic solvents.     

A novel and convenient approach for tosyloxylation of aromatic ring of some ortho-substituted phenolic compounds using [hydroxy(tosyloxy)iodo]benzene

The oxidation of some substituted monohydric phenols, containing electron-withdrawing substituents at the ortho position to the phenolic group, with [hydroxy(tosyloxy)iodo]benzene (HTIB, Koser’s reagent) leads to novel tosyloxylation of aromatic ring, thereby offering a convenient synthesis of hitherto unknown 4-tosyloxy-2-substituted phenols.     

Solvent-free facile synthesis of novel α-tosyloxy β-keto sulfones using [hydroxy(tosyloxy)iodo]benzene

A facile, general and high yielding protocol for the synthesis of novel α-tosyloxy β-keto sulfones is described utilizing relatively non-toxic, [hydroxy(tosyloxy)iodo]benzene, under solvent-free conditions at room temperature.     

Carbon Dioxide in Organic Synthesis: Preparation and Mechanism of Formation of N-(3)-Substituted Hydantoins

The preparation, isolation of intermediates, and the mechanisms of formation of N-(3)-substituted hydantions were investigated. The synthetic pathway involved the reaction of α-aminonitriles with carbondioxide, neat, at room temperature to yield disubstituted ureas and subsequent reaction with water at room temperature to give new N-(3)-substituted hydantoins.     

4,5,6-三取代-2H-吡喃-2-酮的简便合成法

2H-吡喃-2-酮及其衍生物是有机合成的蓬要中间体。对于它们的合成已有许多报道,例如利用烯醇醚或烯醇砖醚与丁酰氯反应;羰基化合物与甲氧亚甲螭丙二酸二甲酯反应;α-苯基丙醛酸酯与丙酮的成环缩合2,6-二氯-3-三氯甲基吡啶与亚甲基丁二酸酯的反应,邻氰基苯乙炔、二苯乙二酮和丙酮的反应。但上述方法往往原料较难得到,产率较低或操作麻烦。     

Efficient Synthesis of 3-Substituted 1,2,4-Triazolo[4,3-a]pyridine by [Bis(Trifluroacetoxy)iodo]benzene-Catalyzed Oxidative Intramolecular Cyclization of Heterocyclic Hydrazones

A series of 1,2,4-triazolopyridines have been prepared by oxidative intramolecular cyclization of heterocyclic hydrazones with [bis(trifluroacetoxy)iodo]benzene. General applicability of this simple transformation was confirmed by synthesis of 1,2,4-triazolo[4,3-a]pyridine. The advantages of this protocol are the nontoxicity of catalyst and shorter reaction time to obtain good preparative yield.