熔融反应合成2,2′-联吡啶桥联二（4,4′-联吡啶）类哑铃型化合物

无溶剂反应;联吡啶;固相熔融;哑铃型化合物     

无溶剂研磨条件下芳基亚甲基麦氏酸的合成

将芳香醛、麦氏酸与NaHCO₃置于研钵中, 在无溶剂存在下通过研磨可以发生缩合反应, 反应产率良好.     

脂肪酶直接与硅胶混合催化无溶剂酯化反应的研究

用硅胶作为载体，以癸酸与己醇的酯化反应作为模型，将脂肪酶和底物直接与硅胶混合，用于无溶剂体系催化酯化反应．结果表明体系中水的含量、底物用量比以及反应时间均对酯化反应有较大影响．在该体系中，脂肪酶催化酯合成反应的速度显著增加，反应2h后．转化率可以达到90％以上．而且沉积在硅胶上的脂肪酶可以反复使用多次．     

无溶剂条件下的有机化学反应．Ⅲ．聚合物史载相转移催化条件下苯酚和卤代烃的反应

无溶剂条件下，以氯型强碱阴离子交换树脂为催化剂，能较好地催化苯酚与卤代烃的反应。     

无溶剂条件下芳香醛与氯代苯乙酮的Darzens 缩合反应

在无溶剂、氢氧化钠的作用下, 用研磨的方法、通过Darzens缩合反应制备环氧化合物. 它的优点是操作简单、反应条件温和、产率高和环境污染小.     

2,2'-联嘧啶衍生物的无溶剂条件合成

2;2'-联嘧啶衍生物的无溶剂条件合成;偶合反应;新鲜铜粉     

微波辐射和加热条件下的无催化剂无溶剂Knoevenagel缩合反应

芳香醛和丙二腈在无催化剂无溶剂存在下在微波辐射或加热条件下可以发生Knoevenagel缩合反应,反应产率良好.     

无溶剂条件下的不对称催化反应

本文综述了近年来在无溶剂条件下进行的一些不对称催化反应的进展, 着重介绍了无溶剂条件下的不对称Aldol反应、环氧化合物不对称开环反应、外消旋环氧化合物的拆分、不对称Diels-Alder反应、金属有机试剂对醛酮的不对称加成反应、不对称氢化反应、不对称氢甲酰化反应、不对称烯烃复分解反应、不对称Michael加成反应、不对称氧化反应、不对称Friedel-Crafts反应等, 同时展望了无溶剂不对称催化反应的研究前景。     

无溶剂条件下香豆素类化合物的绿色合成

以乙酰乙酸乙酯和间苯二酚为原料,固体NaHSO_4·H_2O为催化剂,无溶剂条件下通过Pechmann反应合成7-羟基-4-甲基香豆素;并对反应温度、反应时间、催化剂用量、原料配比等因素对产率的影响进行了探究。实验证明,在无溶剂条件下,NaHSO_4·H_2O是合成7-羟基-4-甲基香豆素的良好催化剂,正交实验法得出反应的最优条件为:反应温度为110℃,反应时间40 min,n(间苯二酚)/n(乙酰乙酸乙酯)=1∶1.2,催化剂用量相对于间苯二酚用量的20%mol,产品的收率为81.8%。     

无溶剂条件下方便、有效的方法合成3-氰基-2-吡啶酮衍生物

芳醛、丙酮和氰乙酰胺为原料,氢氧化钠为催化剂,在无溶剂条件下加热反应有效地合成2-吡啶酮衍生物,本方法具有反应时间短、条件温和、处理简单和环境友好等优点.     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.