一种以三聚氯氰为桥基的新型小分子功能活性染料的合成

以对氨基苯甲酸甲酯和水合肼为原料,经酰胺化反应制得对氨基苯甲酸甲酰胺,进一步与水杨醛通过还原氨化反应生成席夫(1）;以罗丹明B和水合肼为原料,1经闭环反应制得罗丹明B酰肼（2）; 2在四氢呋喃溶剂中与三聚氯氰经缩合取代反应生成一缩产物（3）; 3进一步在四氢呋喃中与1于45~50 ℃回流6 h,经取代反应生成二缩产物,其结构经¹H NMR, MS, IR和元素分析表征。     

新型对叔丁基杯[4]芳烃1,3-二酮衍生物的合成

以对叔丁基苯酚为起始原料,经聚合反应得对叔丁基杯[4]芳烃(2);2经醚化和缩合反应合成了一个新型的对叔丁基杯[4]芳烃1,3-二酮衍生物,其结构经1H NMR,13C NMR和MS表征。     

金丝桃素的合成工艺改进

以大黄素为原料,经还原,Aldol缩合和光照反应合成了金丝桃素,总收率58.6%,其结构经1H NMR, IR和MS表征.     

三苯胺亚胺类化合物的合成

以三苯胺为起始原料,经硝化、还原和胺醛缩合反应合成了4个三苯胺亚胺类化合物,其结构经1H NMR和IR确证。     

富马酸奈拉西坦的合成工艺改进

报道了一种合成富马酸奈拉西坦(7)的新工艺。以衣康酸二甲酯和苄胺为起始原料,经Michael加成和分子内环合反应制得1-苄基-5-氧代吡咯烷-3-羧酸甲酯(3); 3经NaBH₄还原得1-苄基-4-羟甲基-吡咯烷-2-酮(4); 4经甲磺酰化反应得1-苄基-5-氧代吡咯烷-3-羧酸甲磺酸酯(5); 5经氨解得奈拉西坦(6); 6与富马酸经成盐反应合成7,总收率78.4%,其结构经¹H NMR确证。     

新型5＇-脱氧核苷衍生物的合成

以1,2,3-O-三乙酰基-5-脱氧核糖和6-氯嘌呤为主要原料,经Silyl反应制得6-氯-9-(2,3-二-O-乙酰基-5-脱氧-β-D-呋喃核糖)嘌呤(1);1经水解或与亲核试剂经取代和水解反应合成了5个未见文献报道的6-取代-5’-脱氧核苷衍生物,其结构经1H NMR和MS表征。     

1,8-二甲氧基乙基萘的合成

以1,8-二萘酸酐为原料,经氢化铝锂还原得1,8-二羟甲基萘(2);2经浓盐酸酸化生成1,8-二氯甲基萘(3);3经氢化铝锂还原为1,8-二甲基萘(4);用强碱丁基锂和叔丁醇钾将4转化成二钾盐后与甲氧基氯甲烷反应合成了1,8-二甲氧基乙基萘,其结构经1H NMR和13C NMR和HR-MS表征.     

一锅法合成缩氨硫脲类化合物

香草醛和肼基二硫代甲酸甲酯经一锅法合成了两个新的缩氨硫脲类化合物,其结构经UV, 1H NMR, IR和元素分析表征.     

吡啶基三唑功能化罗丹明化合物的合成

以2-溴甲基吡啶氢溴酸盐和叠氮化钠为原料,合成中间体2-叠氮甲基吡啶（1）;对羟基苯甲醛和溴丙炔经取代反应合成中间体4-（丙-2-炔基丙氧基）苯甲醛（2）; 2与1经点击反应制得关键中间体BPT（3）; 3与罗丹明B酰肼经还原胺化反应得罗丹明类荧光探针,其结构经¹H NMR, IR和元素分析表征。     

6-硝基胡椒酸的合成

胡椒醛经硝化,氧化,合成了6-硝基胡椒酸。其结构经UV,IR和MS确认,总收率44％。     

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.     

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.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.