几种手性α-乙酰氨基-β-芳基丙烯酸类化合物的合成

以乙酰甘氨酸和苯甲醛及其衍生物为原料，合成了一系列含碳碳双键的前手性底物，（Z）－2－乙酰氨基苯丙烯酸，（Z）－2－乙酰氨基－3－（对甲氧苯基）－丙烯酸，（Z）－2－乙酰氨基－3－（对氯苯基）－丙烯酸，（Z）－2－乙酰氨基－3－（间氯苯基）－丙烯酸，（Z）－2－乙酰氨基－3－（间硝基苯基）－丙烯酸。后4种是新的有机化合物，产物结构经过核磁共振，质谱分析确证。     

2-氨基-4-芳基噻唑的合成

以苯乙酮（对硝基苯乙酮）、硫脲和碘为原料合成了２－氨基－４－苯基噻唑和２－氨基－４－对硝基苯基噻唑。以α－卤代－２,４－二氯苯乙酮和硫脲为原料合成了２－氨基－４－（２,４－二氯苯基）噻唑。第二种合成方法反应简便,收率高     

2—氨基—5—硝基噻唑的合成研究

以乙酸乙烯酯为原料，经氯化、水解与硫脲环合反应制备2－氨基噻唑，收率91％。将其在硫酸体系中，经成盐－硝化“一锅法”合成2－氨基－5－硝基噻唑。当反应物n（2－氨基噻唑）：n（硫酸）：n（硝酸）＝1：4：1．05，30℃反应4小时，硝化产物收率为81％。     

4—氨基—4’—氯二苯甲酮的合成研究

以Na2S2为还原剂，将4－硝基－4’－氯二苯甲酮还原成4－氨基－4’－氯二苯甲酮，通过对反应物配比、反应时间、反应温度进行多因素正交试验，确定了最佳工艺条件，反应温度92℃，反应时间2．5小时，4－硝基－4’－氯二苯甲酮：Na2S2＝1：1．7（mol），收率为85．80％，含量为98．08％。产品结构经红外光谱、核磁共振、质谱和元素分析证实。实验操作简单，分离容易。     

2-氨基-6-硝基苯并噻唑的合成研究

研究了以对硝基苯胺为原料，在催化剂的作用下，合成2－氨基－6－硝基苯并噻唑。其适宜的工艺条件为：n（对硝基苯胺）：n（硫氰酸胺）：n(苯）＝1：1．15：6．5，反应温度为80－85℃，反应时间为10h；n(对硝基苯基硫脲）：n(催化剂）＝1：0．093，室温反应，反应时间为2h。产品收率为64．5％，纯度≥99％。     

合成4-氨基安替比林类试剂的新途径

4-氨基安替比林属于吡唑酮杂环类化合物,含-CC-、-CO、-NH3个官能团,可望形成具有一定长度、至少含O、N2种配位原子的有机试剂.由于吡唑酮环的稳定性,-CC-、-CO作为反应中心具有一定的局限性,因此有关的反应多发生在4位氨基上.已报道的合成方法有芳香醛与4-氨基安替比林的席夫碱反应、重氮盐反应、成硫脲反应、成酰胺反应等类型.通过4位氨基与卤代烃进行亲核取代,合成新试剂的路线尚未见报道.为此,我们选择芳环上连有硝基的卤代烃与4-氨基安替比林在适当的条件下反应,合成了3种新化合物,对4-氨基安替比林类试剂合成进行了成功的尝试.     

5-(4″,4″,4″-三氟-1″,3″-丁二酮基)-2,2′-联噻吩的合成与性质研究

经酰化、缩合反应,合成得到1种新型β二酮配体5－（4″,4″,4″-三氟－1″,3″－丁二酮基）－2,2′－联噻吩,探讨合成条件对反应的影响,并研究了该β－二酮配体的紫外可见光谱和红外光谱性质。     

4，4‘—二氨基二苯胺—2—磺酸的合成工艺改进

以对硝基氯苯和对硝基苯胺为原料合成4，4‘-二氨基二苯胺－2－磺酸，可大大降低原材料成本，而且均在常压下反应，对生产设备无特殊要求。     

4-(N-乙基,N-2-羟乙基)氨基苯甲醛的制备

以4－（N－乙基，N－2－羟乙基）氨基苯为起始原料经乙酸酐酯化，苯环对位甲酰化，再水解制得4－（N－乙基，N－2－羟乙基）氨基苯甲醛，每步反应平衡，并用TLC跟踪每一步反应进行的程度，总收率达60％。     

2—氨基—1—[（4—苄氧基—3—硝基）苯基]乙醇的合成

合成了4－苄氧基－3－硝基－α－氨基苯乙酮及2－氨基－1－[（4－苄氧基－3－硝基）苯基]乙醇两个未见文献报道的新化合物，该合成方法简便，收率高。     

Comprehensive and Facile Synthesis of Some Functionalized Bis-Heterocyclic Compounds Containing a Thieno[2,3-b]thiophene Motif

A comprehensive and facile method for the synthesis of new functionalized bis-heterocyclic compounds containing a thieno[2,3-b]thiophene motif is described. The hitherto unknown bis-pyrazolothieno[2,3-b]thiophene derivatives 2a-c, bis-pyridazin othieno[2,3-b]thiophene derivatives 4, bis-pyridinothieno[2,3-b]thiophene derivatives 6a,b, and to an analogous bis-pyridinothieno[2,3-b]thiophene nitrile derivatives 7 are obtained. Additionally, the novel bis-pyradazinonothieno[2,3-b]thiophene derivatives 9, and nicotinic acid derivatives 10, 11 are obtained via bis-dienamide 8. The structures of all newly synthesized compounds have been elucidated by (1)H, (13)C NMR, GCMS, and IR spectrometry. These compounds represent a new class of sulfur and Nitrogen containing heterocycles that should also be of interest as new materials.     

Palladium (0) catalyzed Suzuki cross-coupling reactions of 2,4-dibromothiophene: selectivity,characterization and biological applications

A series of novel 2-aryl¹-4-bromothiophenes (2a–f), biarylthiophenes with non-identical aryl groups (3a–e) and biarylthiophenes with identical aryl groups (4a–f) were synthesized in moderate to excellent yields by using different arylboronic acids in a Suzuki–Miyaura cross-coupling reaction. The experimental results showed that the use of K₂CO₃ as base resulted in moderate yields compared with that of good yields obtained upon using K₃PO₄. The highest yield obtained using K₃PO₄ was 82% for 2, 4-bis (4-chlorophenyl) thiophene (4d). The synthesized compounds in the present study were examined for their biofilm inhibition and hemolysis assay. Among all compounds 2, 4-bis (4-methoxyphenyl) thiophene (4b) was found to strongly inhibit the formation of bacterial biofilm against E. coli. The compound 4b exhibited higher inhibition (80.92%) compared with the standard Rifampicin with 97.43% inhibition. The compound 2, 4-bis (4-chlorophenyl) thiophene (4d) displayed strong anti-biofilm activity with its ability to prevent the formation of Pasteurell amultocida biofilm at the percent inhibition of 74.53%. In addition, 2f showed the highest percentage hemolysis 16.0% compared with that of the standard Triton-X-100. 3     

新型噻吩基二醛及其缩氨基硫脲的合成

所合成的２，５－二（２－甲酰苯氧甲基）噻吩２及其缩氨基硫脲化合物２，５－二［（２’－甲酰缩氨硫脲基）苯氧甲基］噻吩３尚未见文献报道。对二者进行了元素分析、红外光谱、氢核磁共振谱、质谱及紫外－可见光谱表征。     

The synthesis and characterization of new organosoluble long chain-substituted metal-free and metallophthalocyanines by microwave irradiation

The long chain-substitued phthalonitrile (3) was synthesized by nucleophilic displacement of nitro group in 4-nitrophthalonitrile with N,N-bis[2-(2-hyroxyethoxy)ethyl]-4-methylbenzenesulfonamide (1). The novel metal-free phthalocyanine (4) and metallophtalocyanines (5–8) have been synthesized by cyclotetramerization reaction of phthalonitrile derivative (3). Long chain-substituted Pcs showed the enhanced solubility in organic solvents. The new compounds were characterized by a combination of IR, ¹H NMR, ¹³C NMR, UV–Vis, elemental analysis and MS spectral data.     

A Novel and Expedient Approach to New Thiazoles, Thiazolo[3,2-a]pyridines, Dihydrothiophenes, and Hydrazones Incorporating Thieno[2,3-b]thiophene Moiety

This paper reports details about the synthesis of a series of novel functionalized symmetrical bis-heterocyclic compounds containing a thieno[2,3-b]thiophene motif. Bis-thiazole derivatives 2, 3a-c and thiazolo[3,2-a]pyridine derivatives 4a-c are achieved. The hitherto unknown dihydrothiophene derivatives 6a-dvia bis-pyridimium salt 5 are obtained. Additionally, the novel hydrazonothieno[2,3-b]thiophene derivatives 10a-c are obtained via bis-tosylacetylthieno[2,3-b]thiophene derivative 9. All compounds are characterized by (1)H-, (13)C-NMR, GCMS, IR, and UV-vis spectrometry. These compounds represent a new class of sulfur and nitrogen containing heterocycles that should also be of interest as new materials.     

Synthesis and Characterization of Polyacetylene with Side-chain Thiophene Functionality

A new polyacetylene derivative with electroactive thiophene substituent, namely poly(2-methylbut-2-enyl thiophene-3-carboxylate) was synthesized and characterized. For this purpose, novel acetylene monomer was synthesized by the reaction of 3-thiophenecarboxylic acid with propargyl bromide and polymerized with a Rh catalyst to give the corresponding polymer. The chemical structure of the polymer was characterized to comprise the conjugated backbone and electroactive thiophene side group. UV spectral changes of the polymer with temperature were also studied. The polymer exhibited better thermal stability than the unsubstituted polyacetylenes.     

Microwave‐Assisted Quick Synthesis of Some Potential High Explosives

This paper reports a novel microwave‐assisted method for the synthesis of potential high explosives (HEs) such as 3‐nitro‐1,2,4‐triazol‐5‐one (NTO), bis‐(2,2‐dinitropropyl) nitramine (BDNPN), 4‐nitroimidazole (4‐NI) and 2,4,6,8,10,12‐hexanitro‐2,4,6,8,10,12‐hexaazaisowurtzitane (CL‐20). The high temperature thermal rearrangement of 1,4‐dinitroimidazole to 2,4‐dinitroimidazole was also reported using microwave radiation as heating source. The synthesized compounds were characterized by spectroscopic techniques and the data obtained confirmed their structures.     

Effect of Lateral Nitro Groups on the Properties of Sulfur-Ligated Twin Mesogens

The syntheses and the properties of new sulfurligated liquid crystalline sulfones, containing biphenyl units, as well as the influence of lateral nitro groups on their phase behaviour are described. Differential scanning calorimetry, optical polarizing microscopy and X-ray diffraction measurements reveal liquid crystalline properties for most of the synthesized bis(4-alkoxy-biphenyl-3-yl)sulfones ( 4 ). The mesomorphic behaviour of these compounds is compared with that of the corresponding nitro compounds 6 . The bis(4-alkoxy-6-nitrobiphenyl-3-yl)sulfones ( 6 ) are not mesogenic. The results demonstrate that lateral nitro groups introduced into the biphenyl unit, changing the length-breadth relation, depress the thermal stability and lead to the loss of the mesomorphic properties.     

Design and Synthesis of Highly Active Peroxisome Proliferator‐Activated Receptor (PPAR) β/δ Inverse Agonists with Prolonged Cellular Activity

Based on 3‐(((4‐(hexylamino)‐2‐methoxyphenyl)amino)sulfonyl)‐2‐thiophenecarboxylic acid methyl ester (ST247, compound 2 ), a recently described peroxisome proliferator‐activated receptor (PPAR)β/δ‐selective inverse agonist, we designed and synthesized a series of structurally related ligands. The structural modifications presented herein ultimately resulted in a series of ligands that display increased cellular activity relative to 2 . Moreover, with methyl 3‐(N‐(2‐(2‐ethoxyethoxy)‐4‐(hexylamino)phenyl)sulfamoyl)thiophene‐2‐carboxylate (PT‐S264, compound 9 u ), biologically relevant plasma concentrations in mice were achieved. The compounds presented in this study will provide useful novel tools for future investigations addressing the role of PPARβ/δ in physiological and pathophysiological processes.     

2-(4-氨基苯基)-5-(2-烷氧基苯基)-1,3,4-(噁)二唑的合成及表征

以对硝基苯甲酸和水杨酸甲酯为起始原料合成了两种新的1,3,4-噁二唑类化合物——2-(4-氨基苯基)-5-(2-乙氧基苯基)-1,3,4-噁二唑和2-(4-氨基苯基)-5-(2-戊氧基苯基)-1,3,4-噁二唑。合成过程中,1,3,4-噁二唑化合物上的硝基采用钯碳催化氢化的方法还原成氨基,使后处理变得容易,产率显著提高,分别达98.4%和96%。通过IR和1HNMR确证了相关化合物的结构。