硒催化羰基化合成苯并噻唑-2-氨基甲酸酯

以非金属Se为催化剂,以CO替代剧毒光气及其复杂衍生物作羰基化试剂,以O2为氧化剂,经2-氨基苯并噻唑与醇发生"一锅法"的硒催化氧化羰基化反应,开辟了一条经济、绿色、简便、高效的合成苯并噻唑-2-氨基甲酸酯类化合物的新途径.研究了反应温度、压力、醇的用量及碱的种类等因素对生成苯并噻唑-2-氨基甲酸酯的影响,获得了实施该...     

2-巯基苯并噻唑衍生物的合成进展

2-巯基苯并噻唑具有很好的经济价值.为了增强和完善2-巯基苯并噻唑的应用性能,通过将其作为一种中间体,与油溶性基团的活性元素结合在同一分子内,开发和研究了其一系列新型的具有良好性能的衍生物,可用作配体、染料、硫化促进剂、蛋白质酶抑制剂以及杀菌、除草和抗病毒药物.对通过包括苯环、巯基上的S、杂环上的N等3个位置上的取代或加成来合成这些衍生物的简单可行方法进行了综述.     

2-取代苯并噻唑化合物的合成进展

2-取代苯并噻唑在生物医药、材料科学等领域的应用和研究使其合成方法受到了广泛的关注.在传统合成方法的研究基础之上,单质硫介导的氧化还原反应和饱和化合物的脱氢芳构化反应等新方法的发展,为苯并噻唑衍生物的合成提供更多可能.此外,近年来新型金属-有机骨架催化剂、组合离子液体/凝胶、超声以及微波辅助等的应用,极大地丰富了苯并噻...     

微波辐射法合成2-(4-取代苯乙烯基)苯并噻唑

甲基苯并噻唑;芳香醛;微波辐射法合成2-(4-取代苯乙烯基)苯并噻唑     

2-二氟溴甲基-1,3-苯并噻唑的简便合成

本文应用二氟溴乙酸作为二氟溴甲基的合成子,实现了2 巯基芳胺与二氟溴乙酸的缩合反应合成2-二氟溴甲基-1,3-苯并噻唑。该反应以5当量二氟溴乙酸,氯苯为溶剂,于100 ℃下与2-巯基芳胺反应18~40 h,产率高达88%。目标产物通过核磁共振和高分辨质谱表征。该反应条件温和,是对现有合成2-二氟溴甲基-1,3-苯并噻唑的良好补充。     

无溶剂条件下离子液体[Hnmp]HSO4催化一锅法合成2 -氨基苯并噻唑-芳甲基-2-萘酚

以离子液体[Hnmp]HSO₄为催化剂, 在无溶剂条件下催化芳香醛、2-氨基苯并噻唑和2-萘酚合成一系列的2 -氨基苯并噻唑-芳甲基-2-萘酚. 该方法条件温和, 反应时间短, 产率高和对环境友好. 此外催化剂可以方便地回收, 且循环使用四次其催化活性并没有显著降低. 目标产物经过了¹H NMR, IR, MS和元素分析确证.     

N-取代苯基-N′-[6-(2-甲基苯并噻唑)基]脲类化合物的合成

以 2 -甲基苯并噻唑和取代苯胺为原料 ,合成了 7个 N-取代苯基 -N′-[6-( 2 -甲基苯并噻唑 )基 ]脲类新化合物 ,产率分别为 82 .0 % ,88.5% ,87.0 % ,90 .5% ,91 .0 % ,83.5%和 85.0 %。其结构经元素分析、IR和1 H NMR确定。     

2-芳基乙烯基苯并噻唑的催化合成及其紫外光谱的取代基效应

甲基苯并噻唑;固相催化剂;缩合反应;2-芳基乙烯基苯并噻唑的催化合成及其紫外光谱的取代基效应     

2-取代苯并噻唑类化合物的合成研究进展

作为生物的二级代谢产物中常见的结构单元,2-取代苯并噻唑及其衍生物在医药、农业等领域有非常广泛的应用。该类化合物的合成备受广大研究者的关注。经过多年的发展,合成此类化合物的方法已比较成熟。本文通过比较目前报导的各种合成方法,按照合成原料的不同进行了分类和总结。此外,还分析了各种合成方法的不足和缺陷,并对此类化合物的合成研究前景进行了展望。     

1-(2-苯并噻唑基)-3-苯基吡唑啉类化合物的合成

有机荧光化合物有多种结构类型,其中含氮唑系杂环类化合物可作为一些合成纤维和塑料制品的增白剂^[1～4]。据此,我们合成了一系列新的具有不同取代基的苯并噻唑基吡唑啉化合物,并观察了其荧光性质。     

The behavior of 2-chloroquinoline-3-carbaldehyde and 2-oxoquinoline-3-carbaldehyde toward stabilized methylenetriphenylphosphoranes and secondary amines

In this study use was made of the Wittig carbonyl olefination reaction and stereo-identification of the resulting alkenes. Condensation of 2-chloroquinoline-3-carbaldehyde with some selected stabilized phosphonium ylides yielded a mixture of the corresponding E and Z olefins in each case. On the other hand reaction of 2-oxoquinoline-3-carbaldehyde with the selected ylides afforded the respective olefins only in one of the possible stereoisomers. The reaction of 2-chloroquinoline-3-carbaldehyde with acetylmethylenetriphenylphosphorane produced the respective olefine together with acridin-3-ol. Heating of (E) and/or (Z)-methyl 3-(2-chloroquinolin-3-yl)acrylate with hydrazine hydrate yielded the corresponding propan-1-ol derivative. Dechlorination of (E)-ethyl 3-(2-chloroquinolin-3-yl)acrylate and/or (E)-4-(2-chloroquinolin-3-yl)but-3-en-2-one was effected upon treatment with morpholine or piperidine in absolute ethanol to give the respective enone derivatives.     

4-羟基-5，8-二甲氧基-萘-2-甲醛的合成

以2,5-二甲氧基苯甲醛为起始原料合成出了软毛柿木中分离到的天然产物4-羟基-5,8-二甲氧基-萘-2-甲醛,原料经过Stobbe缩合,环化,还原,氧化四步生成产物,并对醇选择性氧化成醛的过程进行了详细的研究．整个合成总的产率为32．2％．     

Structure of Molybdenum Complex of Benzothiazole－2－thiolate（η~5－C_5H_5）Mo（CO）_2（C_7H_4NS_2）

ＳｔｒｕｃｔｕｒｅｏｆＭｏｌｙｂｄｅｎｕｍＣｏｍｐｌｅｘｏｆＢｅｎｚｏｔｈｉａｚｏｌｅ－２－ｔｈｉｏｌａｔｅ（η~５－Ｃ_５Ｈ_５）Ｍｏ（ＣＯ）_２（Ｃ_７Ｈ_４ＮＳ_２）ＣｈｅｎｇＧｕｏ－Ｂａｏ~ａ；ＷｕＱｉａｎｇ－Ｊｉｎ~ｂ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ~...     

氨基硫脲缩(4-醛基吡啶)氟硅酸盐的合成和晶体结构

氨基硫脲缩(4-醛基吡啶)4-C5H4NCHNNHCSNH2(HL)和氟硅酸钾K2S iF6反应制备了标题化合物[H(4-C5H4NCHNNHCSNH2)]2S iF6.2H2O(1),用元素分析和X射线单晶衍射对其结构进行了表征.结构解析表明,化合物1属于单斜晶系,P21/c空间群,晶胞参数为:a=0.674 3(2)nm,b=1.349 6(3)nm,c=1.235 7(3)nm,β=94.283(4),°V=1.121 4(5)nm3,Z=2,Mr=540.61,Dc=1.607 g/cm3.μ=0.371 mm-1,F(000)=560,R1=0.036 8,wR2=0.105 4.该化合物由质子化的正一价氨基硫脲缩(4-醛基吡啶)阳离子和氟硅酸根阴离子以及水分子组成.     

Synthesis of spirooxindole analogues from 2-cyclopropyl-4-(4-fluorophenyl)quinoline-3-carbaldehyde

Abstract

A series of spirooxindoles have been synthesized through 1,3-dipolar cycloaddition of an azomethine ylide generated from isatin and sarcosine or L-proline with the dipolarophile (E)-3-(2-cyclopropyl-5-(4-fluorophenyl) quinolin-3-yl)-1-phenylprop-2-en-1-one derivatives. The stereochemistry of the cycloadducts was assigned based on the single-crystal X-ray.     

Characteristic features of intra- and intermolecular interactions in crystals of pyrrole-2-carbaldehyde isonicotinoylhydrazone and its hydrate

Pyrrole-2-carbaldehyde isonicotinoylhydrazone (1) and its hydrate [1·H₂O] (2) were studied by single-crystal X-ray diffraction analysis. The introduction of the pyrrole substituent into N"-substituted isonicotinic hydrazide (INH) causes the intramolecular redistribution of the electron density compared to those in INHs studied earlier, which increases the basicity of the hydrazone nitrogen atom (N") involved in intermolecular hydrogen bonding. This effect has not been observed in the structures of N"-substituted INHs and benzhydrazides studied previously. Intermolecular hydrogen bonds play a decisive role in the formation of the crystal structures of 1 and 2.     

Synthesis and structures of monomeric [chloro(isatin-3-thiosemicarbazone)bis(triphenylphosphine)]copper(I) and dimeric [dichlorobis(thiophene-2-carbaldehyde thiosemicarbazone)bis(triphenylphosphine)]dicopper(I)] complexes

Reaction of copper(I) chloride with thiophene-2-carbaldehyde thiosemicarbazone (Httsc) in acetonitrile in the presence of Ph₃P yielded a sulfur-bridged dimer [Cu₂Cl₂(μ₂-S-Httsc)₂(PPh₃)₂] · 2CH₃CN (1), while a similar reaction with isatin-3-thiosemicarbazone (H₂itsc) formed a monomer, [CuCl(H₂itsc)(Ph₃P)₂] · 2CH₃CN (3). Furan-2-carbaldehyde thiosemicarbazone (Hftsc) also formed a compound of the composition [Cu₂Cl₂(Hftsc)₂(PPh₃)₂] · 2H₂O (2). Complexes 1–3 have been characterized using elemental analysis, IR, ¹H and ³¹P NMR spectroscopy and single crystal X-ray crystallography (1 and 3). Acetonitrile is engaged in hydrogen bonding with the chlorine atom {NCCH₂–H?Cl)}, which is necessary for the stabilization of the bridging sulfur in 1. In compound 3, however, acetonitrile is strongly hydrogen bonded to the NH hydrogen of the isatin ring {CH₃CN?NH(isatin)} and not to the chlorine atom. The Cu?Cu contact of 2.7719(5) Å in dimer 1 is close to twice the van der Waals radius of the Cu atom (2.80 Å).     

Three-component one-pot synthesis of quinoline–furan conjugates from acetylenedicarboxylate,isocyanide, and 2-chloroquinoline-3-carbaldehyde

We have developed a facile and efficient method for the synthesis of functionalized novel furylquinolines. A variety of quinoline–furan conjugates were obtained via the condensation of 2-chloroquinoline-3-carbaldehyde with acetylenecarboxylates and isocyanides in good to excellent yields.     

In situ FTIR study of pyridine-3-carbaldehyde adsorption on TiO2 (anatase) and V-Ti-O catalyst

In situ FTIR spectroscopy was used to study the interaction of pyridine-3-carbaldehyde (3PyA) with the surface of ТiO₂ and a V-Ti-O catalyst in the temperature range of 120-300°C. 3PyA interacts with Lewis and Br?nsted acid sites of ТiO₂ and the V-Ti-O catalyst to form a nitrogen-coordinated complex and a s-bonded (through oxygen of the CHO group) complex, as well as a complex protonated at the N atom in the ring. Surface carboxylates (nicotinates) were also identified during the interaction of 3PyA with the V-Ti-O catalyst in the temperature range of 200-300°C. This revised version was published online in June 2006 with corrections to the Cover Date.     

Synthesis and antimicrobial activity of Schiff bases derived from 2-chloro quinoline-3-carbaldehyde and its derivatives incorporating 7-methyl-2-propyl-3H-benzoimidazole-5-carboxylic acid hydrazide

A series of Schiff bases consisting of two heterocyclic rings derived from 2-chloro quinoline-3-carbaldehyde and its derivatives incorporating 7-methyl-2-propyl-3H-benzoimidazole-5-carboxylic acid hydrazide have been accomplished and thoroughly characterized by various spectroscopic techniques including IR, MS, and multinuclear NMR. These compounds were screened for antimicrobial activity against Escherichia coli, Staphylococcus aureus, Salmonella typhi, and Candida albicans. The derivatives exhibited moderate activity against E. coli and C. albicans.