共查询到19条相似文献,搜索用时 171 毫秒
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以3-硝基-2-氨基苯甲酸甲酯为原料,经三氟乙酰化、N-烷基化和脱保护反应制得坎地沙坦中间体2-{[(2'-氰基联苯基-4-基)甲基]氨基}-3-硝基苯甲酸甲酯,其结构经~1H NMR,~(13)C NMR和MS(ESI)确证。 相似文献
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YAO Jun-hua 《分析测试学报》2007,(Z1)
2-[[(2′-氰基联苯基)-4-基]甲基]氨基-3-硝基苯甲酸乙酯是生产抗高血压药坎地沙坦酯的中间产物[1],由3-硝基邻苯二甲酸为起始原料,经酯化、卤代、Curtius重排、与2-氰基-4′-溴甲基联苯缩合4步反应制得,合成路线见文献[2-3]。在生产过程中,每一步反应带来的副产物都影响到最终 相似文献
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利用 2 ,3 丁二酮与丙二腈缩合形成双甲基双氰基环并内酰胺 ,经酸性水解得到双甲基环并内酯 ,然后和 (S) ( -) ( 1 苯基乙基 )胺反应生成 1,5 二甲基 2 (S) ( 1′ 苯基乙基 ) 2 氮杂 8 氧杂 -双环 [3 .3 .0 ]辛烷 3 ,7 二酮 ,通过元素分析、红外光谱、核磁共振氢谱和质谱对其结构进行了表征 .用X射线单晶衍射法测定了目标产物的晶体结构 ,结果表明 ,晶体属单斜晶系 ,P2 1 空间群 ,a =0 8777( 18)nm ,b =1 0 10 2 ( 2 )nm ,c =0 90 0 9( 18)nm ,β =118 75 ( 3 )° ,V =0 70 0 3 ( 2 )nm3 ,Dc=1 2 96g·cm-3 ,μ =0 0 89mm-1 ,F( 0 0 0 ) =2 92 ,Z =2 ,R1 =0 0 3 93 ,wR2 =0 0 95 5 . 相似文献
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2-氰基-2,3-二甲基-3-甲基羰甲基-5-硫酮-吡咯烷的合成 总被引:2,自引:0,他引:2
2-氰基-2;3-二甲基-3-甲基羰甲基-5-硫酮-吡咯烷的合成;双甲基环并内酯;双甲基环并内酰胺-内酯;氰基吡咯烷酮;氰基吡咯烷硫酮 相似文献
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庄航 《理化检验(化学分册)》2020,56(4):438-442
建立了气相色谱-串联质谱法测定苯甲酸阿格列汀关键起始物料2-氰基溴苄中基因毒性杂质3-氰基溴苄和4-氰基溴苄含量的分析方法。采用50%苯基-50%二甲基聚硅氧烷为固定液的VF-17MS毛细管柱(30m×0.25mm,0.25μm)进行程序升温;进样口温度260℃;以多反应监测(MRM)模式检测。2种待测物均具有较好的线性关系,相关系数均大于0.998 0;检出限(3S/N)均为2.0μg·L^-1;3-氰基溴苄的回收率为92.1%~97.0%;4-氰基溴苄的回收率为102%~109%;供试品溶液、杂质对照品溶液和系统适用性溶液在室温(25℃)下放置18h内稳定。三批生产规模样品中均未检出3-氰基溴苄和4-氰基溴苄。建立的分析方法灵敏度高、分离度好、结果准确,可有效分离并测定2-氰基溴苄中的3-氰基溴苄和4-氰基溴苄含量,为苯甲酸阿格列汀的安全性提供了保障。 相似文献
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Rodinovskaya L. A. Gromova A. V. Shestopalov A. M. Nesterov V. N. 《Russian Chemical Bulletin》2003,52(10):2207-2213
Substituted 3-hydroxypyrazoles, which were prepared based on ethyl esters of substituted 4-(pyridin-2-ylthio)- or 4-(1,4-dihydropyridin-2-ylthio)acetoacetic acids and hydrazine hydrate, were used in the synthesis of 6-amino-4-aryl-5-cyano-3-(pyridin-2-ylthiomethyl)-2,4-dihydropyrano[2,3-c]pyrazoles. The molecular and crystal structure of 6-amino-5-cyano-3-(3-cyano-4,6-dimethylpyridin-2-ylthiomethyl)-4-(2-nitrophenyl)-2,4-dihydropyrano[2,3-c]pyrazole was established by X-ray diffraction analysis. 相似文献
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James H. Looker Duane L. Shaneyfelt Wayne Halfar 《Journal of heterocyclic chemistry》1979,16(6):1281-1282
Condensation reactions of comenaldehyde methyl ether (I) with malonic acid, ethyl cyanoacetate, and cyanoacetamide to give β-(5-methoxy-4H-pyran-4-on-2-yl)acrylic acid (II), ethyl 2-cyano-3-(5-methoxy-4H-pyran-4-on-2-yl)propenoate (III), and 2-cyano-3-(5-methoxy-4H-pyran-4-on-2-yl)propenamide (IV), respectively, are described. Ultraviolet absorption spectra for 2-hydroxymethyl-5-methoxy-4H-pyran-4-one, I and II are presented. 相似文献
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Aïcha Arfaoui 《Tetrahedron》2009,65(25):4904-4907
A regioselective coupling of ethyl 2-(bromomethyl)-3-cyanoacrylate and primary amines is described to give ethyl 2-[(alkylamino)(cyano)methyl] acrylates in good yields. Whereas the conversion of allyl bromide in the presence of TEAF leads to the first synthesis of ethyl 3-cyano-2-(hydroxymethyl) acrylate. 相似文献
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3-Oxo-2,3-dihydrobenzofuran reacted with ethyl 2-cyano-3-ethoxypropenoate, methyl 2-cyano-3-methoxy-propenoate affording compounds 3 (2-(2-cyano-2-alkoxycarbonylvinyl)-3-hydroxybenzofuran) obtained as a mixture of Z + E isomers. Methyl 2-methoxycarbonyl-3-methoxypropenoate gave compound 4 . Malonic compounds added on 2-dimethylaminomethylene-3-oxo-2,3-dihydrobenzofuran 6 for giving compound 3 or 2-oxo-3-methoxycarbonyl-2H-pyrano[3,2-b]benzofuran 8 . Compound 8 was also obtained by heating compound 4 in xylene. 相似文献
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Ethyl 2-chloroacetoacetate and its 4-chloro isomer react with cyanoacetamide in the presence of the mild, nonnucleophilic base, triethylamine under stoichiometric conditions to give high yields of ethyl 4-cyano-2-hydroxy-2-methyl-5-oxopyrrolidine-3-carboxylate and ethyl (4-cyano-2-hydroxy-5-oxopyrrolidin-2-yl)acetate, respectively. These, under acid-catalyzed dehydration conditions, afforded ethyl 4-cyano-5-hydroxy-2-methyl-1H-pyrrole-3-carboxylate and ethyl (2Z)-(4-cyano-5-oxopyrrolidin-2-ylidene)ethanoate, respectively. Similarly, the 4-chloro isomer reacted with ethyl cyanoacetate to give the novel product, diethyl 2-cyano-4-oxohexanedioate. The use of triethylamine enables access to a whole new library of pyrrole derivatives from easily accessible, commercially available starting materials. The reactions described in this Letter enable access to libraries of important pyrrole systems in any of the isotopically enriched forms. 相似文献
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S. G. Krivokolysko V. D. Dyachenko V. N. Nesterov V. P. Litvinov 《Chemistry of Heterocyclic Compounds》2001,37(7):855-860
The reaction of o-iodobenzaldehyde, cyanothioacetamide, and N-acetoacetyl-o-toluidine in the presence of piperidine gave piperidinium 4,5-trans-3-cyano-6-hydroxy-4-(2-iodophenyl)-6-methyl-5-(2-methylphenyl)carbamoyl-1,4,5,6-tetrahydropyridine-2-thiolate used in the synthesis of substituted 4,5-trans-2-alkylthiotetrahydropyridines and 2-(2-thiazolyl)acrylonitriles. The structure of 3-(2-iodophenyl)-2-(4-phenyl-2-thiazolyl)acrylonitrile was studied using X-ray diffraction structural analysis. 相似文献
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Lyubov' N. Sobenina Vladislav N. Drichkov Al'bina I. Mikhaleva Olga V. Petrova Igor A. Ushakov Boris A. Trofimov 《Tetrahedron》2005,61(20):4841-4849
5-Amino-3-(pyrrol-2-yl)isoxazoles were selectively prepared by the reaction of 2-(2,2-dicyano-1-ethylthioethenyl)pyrroles with hydroxylamine in methanol. Under analogous conditions, 2-(2-carbamoyl-2-cyano-1-ethylthioethenyl) pyrroles with hydroxylamine gave 5-aminoisoxazoles and their structural isomers, 3-aminoisoxazoles (3-5% yield). The latter were selectively prepared by reacting 2-(2-carbamoyl-2-cyano-1-ethylthioethenyl)pyrroles with hydroxylamine in the presence of aqueous NaOH and from the products of intramolecular cyclization of 2-(2-carbamoyl-2-cyano-1-ethylthioethenyl)pyrroles, 1-ethylthio-3-iminopyrrolizines and hydroxylamine. 相似文献
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Condensation of 2-nitrothiophenol with ethyl propiolate afforded 3-(2-nitrophenylthio)propenoate. Oxidation of sulfur atom to sulfone group gave ethyl 3-(2-nitrophenylsulfonyl)propenoate, which underwent condensation with tosyl methylisocyanide (TosMIC) to yield ethyl 4-(2-nitrophenylsulfonyl)pyrrole-3-carboxylate. Reduction of nitro group afforded ethyl 4-(2-aminophenylsulfonyl)-1H-pyrrole-3-carboxylate, which was cyclized to 2H-pyrrolo[3,4-b][1,5] benzothiazepin-10(9H)-one 4,4-dioxide. Similar procedure was used for the synthesis of 9,10-dihydro-10-methyl-2H-pyrrolo[3,4-b][1,5]benzothiazepine 4,4-dioxide. 相似文献
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S. G. Krivokolysko V. D. Dyachenko E. B. Rusanov V. P. Litvinov 《Chemistry of Heterocyclic Compounds》2001,37(8):987-992
4-(2-Chlorophenyl)-3-cyano-6-hydroxy-5-(2-thienoyl)-6-trifluoromethylpiperidin-2-thione, which was used for the synthesis of 2-allylthio-4-(2-chlorophenyl)-3-cyano-6-hydroxy-5-(2-thienoyl)-6-trifluoromethyl-1,4,5,6-tetrahydropyridine, was obtained by the reaction of 2-thienoyltrifluoroacetone with 2-chlorophenylphenylmethylenecyanothioacetamide or with a mixture of 2-chlorobenzaldehyde and cyanothioacetamide in the presence of N-methylmorpholine. The molecular and crystal structure of the piperidinthione have been established by X-ray crystallography. 相似文献