共查询到19条相似文献,搜索用时 125 毫秒
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以丁烯酸和2-巯基噻吩为原料,经加成缩合制得3-(2-噻吩硫基)丁酸(2);以氯化亚砜氯化,三氯化铝催化环合得5,6-二氢-4H-6-甲基噻嗯并[2,3-b]噻喃-4-酮(3);再经磺化、氯化、氨解反应合成得5,6-二氢-4H-6-甲基噻嗯并[2,3-b]噻喃-4-酮-2-磺酰胺(1)。其中经均匀设计优化了环合反应条件为:n(2)∶n(氯化亚矾)∶n(三氯化铝)=1∶3∶1.5,于20℃反应2h。以2-巯基噻吩计,1合成总收率为30.49%,结构经IR、MS、1HNMR确证。 相似文献
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乙酰乙酸乙酯与对甲苯胺、磷酸二氢钾反应得到3-(对甲苯氨基)-2-丁烯酸乙酯(化合物3);4-氨基-1-萘酚盐酸盐与甲氧基苯磺酰氯反应得到4-甲氧基-N-(4-羟基萘)苯磺酰胺(化合物6),之后经高碘酸钠氧化得到4-甲氧基-N-(4-氧代萘)苯磺酰胺(化合物7);中间体3和7发生环化得到目标物2-甲基-5-(4-甲氧基苯磺酰胺)萘并[1,2-b]呋喃-3-羧酸乙酯(化合物8),其结构经1H NMR、13C NMR和HRMS确证.对中间体3、中间体7以及目标物8的合成条件进行优化,滴加原料对甲苯胺、使用KH2PO4作为催化剂时,可在较低温度下顺利得到中间体3;控制氧化剂用量、使用乙醇含量高的水溶液作为溶剂有利于中间体7的生成和后处理;在反应体系中加入少量水,可减少化合物8的副产物生成.该方法为N-(萘并[1,2-b]呋喃-5-基)苯磺酰胺类化合物的合成提供了参考. 相似文献
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Mohamed I. Ali M. Amine Abou-State A. Fouad Ibrahim 《Advanced Synthesis \u0026amp; Catalysis》1974,316(1):147-153
2-Methyl-5,6-diphenyl-2,3-dihydro-imidazo[2,1-b]thiazol-3-one 5 and 6,7-diphenyl-2,3-dihydro-4H-imidazo[2,1-b]1,3-thiazin-4-one 6 are prepared from 4,5-diphenyl-2-mercapto-imidazole 1 . Compounds 5 and 6 react with amines or hydrazines to give the 2-(4,5-diphenyl-imidazol-2-ylthio)acet(or propan) amides (hydrazides) 7a – g and the 3-(4,5-diphenyl-imidazol-2 ylthio) propanamides(hydrazides) 8a – e , respectively. The hydrazides 7a, 7b and 8a are condensed with aromatic aldehydes to the hydrazones 9a – h and 10a – d . Compound 5 couples with aryldiazonium salts to give 2-arylazo-2-methyl-5,6-diphenyl-2,3-dihydro-imidazo[2,1-b]thiazol-3-ones 11a – d . 相似文献
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以2,3-二氨基吡啶或2,3,5,6-四氨基吡啶盐酸盐等为原料合成了吡啶并吡嗪、吡啶并咪唑及吡啶并二咪唑氮杂环衍生物。探讨了反应条件对产物收率的影响,初步确定了优化反应条件。对2,3-二甲基吡啶并吡嗪及2,3-二乙基吡啶并吡嗪的合成,氯化铵-甲醇体系具有明显的催化效果。使用4,5-二羟基咪唑烷-2-酮代替乙二醛与2,3-二氨基吡啶反应,可显著提高吡啶并吡嗪的合成收率;对于吡啶并咪唑和2-甲基吡啶并咪唑的合成,以2,3-二氨基吡啶与原甲酸三乙酯或原乙酸三甲酯为原料,在磷钼酸催化下反应,收率达50%以上;对于吡啶并[2,3-b:5,6-b']二咪唑和2,6-二甲基吡啶并[2,3-b:5,6-b']二咪唑的合成,分别以2,3,5,6-四氨基吡啶盐酸盐与原甲酸三乙酯和原乙酸三甲酯为原料在磷钼酸催化下反应,收率可达68.7%和66.5%。 相似文献
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Dinesh W. Rangnekar 《Journal of chemical technology and biotechnology (Oxford, Oxfordshire : 1986)》1990,49(4):311-320
4-Nitroso-1-phenyl-3-methyl-5-aminopyrazole ( 1 ) was condensed with ethylcyanoacetate ( 2 ), malononitrile ( 4a ) and 2-cyanomethylbenzimidazole ( 4b ) to yield 6-hydroxy-5-cyano, 6-amino-5-cyano and 6-amino-5-(benzimidazol-2-yl)-3-methylpyrazolo [3,4-b]pyrazines 3, 5a and 5b , respectively. 5-Cyano-6-chloro derivative 6 obtained from 3 was converted to 3-aminopyrazolo[4′,3′:5,6]pyrazino[2,3-c]pyrazoles 8a and 8b by the treatment with hydrazin hydrate ( 7a ) and phenylhydrazine ( 7b ), respectively. Compound 5a was treated with formamide ( 9a ), urea ( 9b ) and thiourea ( 9c ) to give 4-aminopyrazolo[4′,3′:5,6]pyrazino[2′3′-d]pyrimidines 10a–10c. With refluxing acetic anhydride compounds 8a, 8b and 10a gave corresponding acetamido derivatives 8c, 8d and 10d. Compound 5a was treated with ethylorthoformate ( 11 ), acetic anhydride ( 12 ) or benzoylchloride ( 13 ) to give fused benzimidazopyrazolo[4′,3′:5,6]pyrazino[2′,3′-d]pyrimidines, viz., benzimidazol[1,2-c]pyrazolo[4,3-g]pteridines ( 14a–14c ). Some of the compounds 8, 10 and 14 were applied to polyester as disperse dyes and their fastness properties were studied. 相似文献
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Mohamed I. Ali A. Bayoumi Mostafa Adly A. Soliman 《Advanced Synthesis \u0026amp; Catalysis》1976,318(1):12-18
5-Aryl-3-carboxymethylthio-1,2,4-triazoles 2 are cyclised to 6-arylthiazolo[3,2-b]-s-triazol-3(2H)-ones 3 . This structural assignment has been based on IR and NMR spectra. 2-Arylmethylene-6-arylthiazolo[3,2-b]-s-triazol-3(2H)-ones 7 were prepared by several methods. Compounds 3 coupled with diazotised anilines to give 2,3-dihydro-6-arylthiazolo[3,2-b]-s-triazole-2,3-dione 2-arylhydrazones 8 . The action of amines on 3a opens the thiazolone ring with the formation of substituted (5-phenyltriazol-3-ylthio)-acetamides 9 . 相似文献
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Derivatives of 2-Phenyl- and 2-Methyl-2,3-dihydro-1,4-dithiine-5,6-dicarboxylic Acid Imide The reaction between 2-phenyl- ( A ) and 2-methyl-2,3-dihydro-1,4-dithiine-5,6-dicarboxylic acid imide ( B ), respectively, and primary aromatic amines or diamines in the presence of formaldehyde or acetaldehyde yields the α-aminoalkyl- and bis-α-aminoalkyl derivatives 1—26 . Interaction of A and B with disulfides, sulfochlorides, sulfuryl chloride, acetanhydride, acid chlorides and chloroformic acid esters affords the N-substituted compounds 27—32, 33—38, 39—40 and 41—48 , respectively. The IR spectra of the products are discussed. 相似文献
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Mabkhot YN Barakat A Al-Majid AM Alshahrani SA 《International journal of molecular sciences》2012,13(2):2263-2275
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. 相似文献
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Poly (3,3-dimethyl-3,4-dihydro-2H-thieno[3,4-b][1,4]dioxepine), PProDOT-Me2, is one of the most promising conducting polymers in the alkylenedioxythiophene based family for electrochromic window applications. In the electropolymerization kinetic study of 3,3-dimethyl-3,4-dihydro-2H-thieno[3,4-b][1,4]dioxepine (ProDOT-Me2), microgravimetry and chronoamperometry were used to determine the reaction orders with respect to the electrolyte and monomer, and the corresponding general kinetic equation of electropolymerization. This study presents that monomer concentration has a strong impact on electropolymerization mechanism. The relationship between film thickness and polymerization time was analyzed indicating that saturation of polymerization reduced the increase rate of film thickness with polymerization time. Also, the electropolymerization conditions were optimized to reach high contrast (Δ%T > 70%) with the minimum of transmittance (%Tmin < 1) for electrochromic window applications. 相似文献
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To investigate the reactions that occur in the flavanoid unit during the liquefaction of tannin in phenol, the phenolysis of (+)-catechin was studied using either H2SO4, HCl, or BF3 2H2O as acid catalyst. In addition to 2-[3-(3,4-dihydroxyphenyl)-2-hydroxy-3-(4-hydroxyphenyl)propyl]-1,3,5-benzenetriol (1) and 2-[(3,4-dihydroxyphenyl)(4-hydroxyphenyl)methyl]-2,3-dihydro-4,6-benzofurandiol (3) that have been described previously, eight additional reaction products were isolated, four of which were compounds that have not been described previously. The novel compounds described here are: 2-[3-(3,4-dihydroxyphenyl)-2-hydroxy-3-(2-hydroxyphenyl)propyl]-1,3,5-benzenetriol (2), 2-[(3,4-dihydroxyphenyl)(2-hydroxyphenyl)methyl]-2,3-dihydro-4,6-benzofurandiol (4), 2-[(3,4-dihydroxyphenyl)(4-hydroxyphenyl)methyl]-2,3-dihydro-7-(4-hydroxyphenyl)methyl-4,6-benzofurandiol (5), and 2-(1,3,5-trihydroxyphenyl)methyl-3-(3,4-dihydroxyphenyl)-6-[(3,4-dihydroxyphenyl)(4-hydroxyphenyl)methyl]-2,3,5,6-tetrahydrobenzo[1,2-b:5,4-b′]-difuran-4-ol (6). The structures of these and other previously described products are consistent with opening of the pyran ring of catechin and reaction at C-2 by either the para or the ortho position of phenol. Additional products resulting from reaction between pyran ring cleavage products and catechin, and from reaction of cleavage products were found. Similar reactions would be expected to take place during the phenolysis of condensed tannins. 相似文献