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以乙醇为溶剂,冰醋酸为催化剂,4-氨基-5-(1-苯基-3-甲基-5-氯吡唑)-1,2,4-三唑-3-硫酮(1)与芳醛经缩合反应合成了7个新型的4-取代苯次甲亚胺-5-(1-苯基-3-甲基-5-氯吡唑)-4H-1,2,4-三唑-3-硫酮(3a~3g),收率66%~74%,其结构经1H NMR,IR及元素分析表征。合成4-(苯次甲亚胺)-5-(1-苯基-3-甲基-5-氯吡唑)-2H-1,2,4-三唑-3-硫酮(3a)的最佳反应条件为:以乙醇为溶剂,乙酸为催化剂,1 10 mmol,n(苯甲醛)∶n(1)=1.2,于75℃反应3 h,产率74%。 相似文献
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报道了四种吡唑衍生物和它们四种新型的杂环酰胺衍生物的合成,它们是3,5-二甲基吡唑(1),5-甲基-3-苯基吡唑(2),3,5-二苯基吡唑(3),5-甲基-3-二茂铁基吡唑(4),2,6-双(3,5-二甲基吡唑基-1-羰基)吡啶(5),2,6-双(5-甲基-3-苯基吡唑基-1-羰基)吡啶(6),2,6-双(3,5-二苯基吡唑基-1-羰基)吡啶(7)和2,6-双(5-甲基-3-二茂铁基吡唑基-1-羰基)吡啶(8).并对它们进行了元素分析,FT-IR,^1H NMR和^13C NMR等波谱分析. 相似文献
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1-芳基-4-吡唑-5-酰基氨基脲类化合物的合成及杀菌活性 总被引:1,自引:0,他引:1
为了寻求新的吡唑先导化合物, 用4-氯-1-甲基-3-乙基-5-吡唑甲酰肼与取代苯基异氰酸酯反应得到了14个新的1-吡唑酰基-4-芳基氨基脲类化合物. 经IR, 1H NMR, MS和元素分析对化合物的结构进行了表征. 初步生物活性实验结果表明, 在500 mg/mL浓度下, 化合物1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-(2-甲基苯基)氨基脲(4g), 1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-(2,4-二甲基苯基)氨基脲(4k)对小麦白粉病菌(Blumeria graminis)的抑制率分别达到90%和80%; 在25 mg/mL浓度下, 化合物1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-苯基氨基脲(4c)对黄瓜灰霉病菌(Botrytis cinerea)的抑制率达到70.1%; 化合物1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-苯基氨基脲(4c)和1-(4-氯-3-乙基-1-甲基-1H-吡唑-5-甲酰基)-4-(2-硝基苯基)氨基脲(4d)对稻瘟病菌(Pyricularia oryzae)的抑制率均达到51.3%. 相似文献
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为实现多种活性成分的有效叠加和为药物筛选提供先导化合物,以1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酸为初始原料,依次合成1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酰氯、1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酰基异硫氰酸酯,再与取代苯并噻唑肼反应生成了8个未见报道的N-取代苯并噻唑-2-氨基-N'-取代吡唑-4-甲酰基硫脲.采用超声波催化法合成了标题化合物,并与加热回流的常规方法进行了对比.超声波催化法具有操作简单、反应时间短、条件温和、产率高、副反应少等优点,为此类化合物的合成提供了一种有效的新方法.标题化合物经元素分析,IR,1HNMR确证结构. 相似文献
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超声辐射下合成1-[(未)取代苯酰基-3-[5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑-2-基]-硫脲 总被引:2,自引:0,他引:2
1-苯基-3-甲基-5-氯吡唑-4-甲酸与氨基硫脲在三氯氧磷中反应得到2-氨基-5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑(1), 然后分别采用超声辐射法和常规加热法与(未)取代苯甲酰基异硫氰酸酯(2)反应合成了一系列未见报到的1-[(未)取代苯酰基-3-[5-(1-苯基-3-甲基-5-氯吡唑-4-基)-1,3,4-噻二唑-2-基]-硫脲(3a~3j). 化合物的结构经元素分析, IR, 1H NMR确证. 相似文献
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5-苯基-1H-3吡唑酰腙化合物的合成及其结构表征 总被引:1,自引:1,他引:0
采用"一锅法"合成了5-苯基-1H-3-吡唑甲酸乙酯,进而合成了9种5-苯基-1H-3-吡唑酰腙化合物,通过元素分析、红外光谱、核磁共振氢谱等测试技术对这9个化合物的结构进行了表征. 将5-苯基-1H-3-吡唑甲酸乙酯水解得到5-苯基-1H-3-吡唑甲酸,此化合物与Cu(AcO)2配位,得到一个铜的三核配合物晶体,该晶体属单斜晶系,空间群为C2/c,晶胞参数为a=2.576 7(3) nm,b=1.1 94 4(1) nm,c=1.412 7(2) nm,β=98.993(2)°,V=4.294 1(9) nm 3,Z=4,Dc=1.629 g/cm 3,R1=0.035 5,结果更进一步确定了吡唑环的结构. 相似文献
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É. S. Krichevskii O. B. Romanova A. N. Grinev 《Chemistry of Heterocyclic Compounds》1983,19(12):1302-1305
Bromination of 2-methyl-3-phenyl-5-nitroindoles has given previously unknown 2-bromoethyl-3-phenyl-5-nitroindoles, which were converted by the Delepine reaction into 2-aminomethyl-3-phenyl-5-nitroindoles. One of these (1-methyl-2-aminomethyl-3-phenyl-5-nitroindole) was also obtained by reductive amination of 1-methyl-2-formyl-3-phenyl-5-nitroindole by the Leuckart-Wallach reaction. 相似文献
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The reaction of 3-methyl-4-oxo-4,5,6,7-tetrahydroindazoles with benzaldehydes gave 5-benzylidene-3-methyl-4-oxo-4,5,6,7-tetrahydroindazoles. Under Mannich conditions, 3-methyl-1-phenyl-4,5,6,7-tetrahydroindazole gave 5-aminomethyl-3-methyl-4-oxo-1-phenyl-4,5,6,7-tetrahydroindazoles. 相似文献
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By a combination of hydrolysis, decarboxylation, and methylation diethyl 1-methyl-3-hydroxy-5-phenylpyrrole-2,4-dicarboxylate was converted into 1-methyl-3-methoxy-5-phenyl-pyrrole-2,4-dicarboxylic acid (5) and into the isomeric compounds ethyl 1-methyl-2-phenyl-4-methoxypyrrole-3-carboxylate (4a) and ethyl 1-methyl-3-methoxy-5-phenylpyrrole-2-carboxylate (9a). 1-Methyl-2-phenyl-4-methoxypyrrole-3-carboxylic acid was synthesized both by the selective decarboxylation of 5 and by the hydrolysis of 4a. Hydrolysis of 9a, however, did not give the corresponding acid, but rather an oxidation product, 1-methyl-3-methoxy-5-hydroxy-5-phenyl-3-pyrrolin-2-onc (10a). Compound 10a was shown to arise from the air oxidation of the completely decarboxylated product, 1-methyl-2-phenyl-4-methoxypyrrole. Reduction of 9a with lithium aluminum hydride gave 1-methyl-3-methoxy-5-phenylpyrrole-2-methanol, which yielded 10a upon oxidation with silver oxide. 相似文献
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N. R. El-Rayyes G. H. Hovakeemian H. Hammoud 《Magnetic resonance in chemistry : MRC》1983,21(4):243-245
The reaction of 1-p-methoxyphenyl-3-phenyl-2-propen-1-one and 3-p-methoxyphenyl-1-phenyl-2-propen-1-one with methylhydrazine gave 1-methyl-3-p-methoxyphenyl-5-phenylpyrazoline and 1-methyl-3-phenyl-5-p-methoxyphenylpyrazoline, respectively. These compounds, on oxidation, gave 1-methyl-3-p-methoxyphenyl-5-phenylpyrazole(2) and 1-methyl-3-phenyl-5-p-methoxyphenylpyrazole, respectively. When methyl-hydrazine was made to react with 1-p-methoxyphenyl-3-phenyl-2-propyn-1-one, a pyrazole was obtained which proved to be identical with 2. Confirmatory evidence for this identity was obtained from their spectral data. 相似文献
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A series of new tweezers amido-amine ligands containing pyrrole, bipyrrole, and dipyrrolylmethane fragments were synthesized by reaction of 2-thioxothiazolidin-3-yl derivatives of α-pyrrolecarboxylic acids {5-[1-(5-carboxy-3-methyl-4-phenyl-1H-pyrrol-2-yl)-1-methylethyl]-4-methyl-3-phenyl-1H-pyrrole-2-carboxylic acid, 5-[(5-carboxy-3-methyl-4-phenyl-1H-pyrrol-2-yl)phenylmethyl]-4-methyl-3-phenyl-1H-pyrrole-2-carboxylic acid, 5-(5-carboxy-3-methyl-4-phenyl-1H-pyrrol-2-yl)-4-methyl-3-phenyl-1H-pyrrole-2-carboxylic acid, and 3,4-dimethyl-pyrrole-2,5-dicarboxylic acid} with o-phenylenediamine. All compounds obtained were characterized by elemental analysis, NMR and mass spectra. 相似文献
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二芳杂环基乙烯的合成及其光致变色反应研究 总被引:2,自引:0,他引:2
本文报道了2,3-双 (1,2-二甲基-3-吲哚基)-2-丁烯 (DF1),2,3-双 (1,4-二苯基-2-甲基-3-吡咯基)-2-丁烯 (DF2), 2,3-双(1-对甲苯基-4-苯基-2-甲基-3-吡咯基)-2-丁烯 (DF3), 2,3-双(1-对溴苯基-4-苯基-2-甲基-3-吡咯基)-2-丁烯 (DF4) 和2,3-双 (1-对甲氧苯基-5-苯基-2-甲基-3-吡咯基)-2-丁烯 (DF5) 的合成,以及它们的光致变色行为的研究。特别是DF1和DF5的光呈色和光消色过程进行了较为细致的研究。 相似文献
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M. S. K. Youssef S. A. M. Metwally M. A. El-Maghraby M. I. Younes 《Journal of heterocyclic chemistry》1984,21(6):1747-1752
1-Phenyl-3-methyl-5-pyrazolone-4-oxime reacted with benzylamine, methylamine, methyl- and ethyl ioides to give 3-methyl-1,5-diphenyl-1H-, 3-methyl-1-phenyl-1H- and 3,5-dimethyl-1-phenyl-1H-pyrazolo[4,3-d]oxazoles I, II. The structure of I was elucidated authentically through other routes by interaction of 1-phenyl-3-methyl-4,5-dioxopyrazolone with benzylamine and/or benzaldehyde and ammonium acetate. Various 3-meth-yl-5-aryl-1-phenyl-1H-pyrazolo[4,3-d]oxazoles IV were synthesized by the reaction of 4,5-dioxopyrazolone with aromatic aldehydes in the presence of ammonium acetate. Also, the structure of I was elucidated authentically via other routes by the reaction of 1-phenyl-3-methyl-4-imino-5-pyrazolone with each of benzylcyanide, benzylamine, benzaldehyde and benzalaniline. 相似文献
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Diethyl 1-methyl-3-hydroxy-5-phenylpyrrole-2,4-dicarboxylate has been synthesized in good yield from readily available materials, diethyl benzylidenemalonate and ethyl sarcosinate. It was found to react with oxygen in aqueous base to give two oxidation products, ethyl 1-methyl-2-oxo-3-hydroxy-5-phenyl-3-pyrroline-4-carboxylate ( 9 ) and ethyl 1-methyl-2,3-dioxo-5-phenyl-4-pyrroline-4-carboxylate ( 10 ). These two oxidation products are postulated to arise from the decomposition of a common intermediate, diethyl 1-methyl-2-hydroperoxy-3-oxo-5-phenyl-4-pyrroline-2,4-dicarboxylate. Reaction of the title compound with oxygen in pyridine containing Triton B again produced two products, the dioxo compound ( 10 ) and diethyl 1-methyl-2-hydroxy-3-oxo-5-phenyl-4-pyrroline-2,4-dicarboxylate ( 12 ). Compound 12 was shown to react in aqueous base to give exclusively 9 . The hydration of 10 in acidic and basic media is also discussed. 相似文献
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Gordon W. Gribble Erin T. Pelkey Wendy M. Simon Hernando A. Trujillo 《Tetrahedron》2000,56(52):10133-10140
The unsymmetrical mesoionic münchnones 13 (3-benzyl-2-methyl-4-phenyl-1,3-oxazolium-5-olate) and 14 (3-benzyl-4-methyl-2-phenyl-1,3-oxazolium-5-olate) react with the N-protected 2- and 3-nitroindoles 1 (ethyl 2-nitroindole-1-carboxylate), 6 (3-nitro-1-(phenylsulfonyl)indole), and 17 (ethyl 3-nitroindole-1-carboxylate) in refluxing THF to afford in good to excellent yields the pyrrolo[3,4-b]indoles 15 (2-benzyl-1-methyl-3-phenyl-4-carboethoxy-2,4-dihydropyrrolo[3,4-b]indole), 16 (2-benzyl-3-methyl-1-phenyl-4-carboethoxy-2,4-dihydropyrrolo[3,4-b]indole), 18 (2-benzyl-1-methyl-3-phenyl-4-(phenylsulfonyl)-2,4-dihydropyrrolo[3,4-b]indole), and 19 (2-benzyl-3-methyl-1-phenyl-4-(phenylsulfonyl)-2,4-dihydropyrrolo[3,4-b]indole). In several cases the regiochemistry, which is opposite to that predicted by FMO theory, is very high and leads essentially to a single pyrrolo[3,4-b]indole; e.g., 6+13→19 in 74% yield. 相似文献
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铽与4—酰代吡唑啉酮—5的三元配合物的合成与荧光性质 总被引:4,自引:0,他引:4
合成并表征了一系列铽与含不同4-酰代的1-苯基-3-甲基-吡唑啉酮-5的三元配合物Tb9L)3.2H2O和Tb(L)3.Dipy「L=1-苯基-3-甲基-4-乙酰基吡啥林酮-5(PMAP),1-苯基-3-甲基-4-丙酰基吡唑啉酮-5(PMPP),1-苯基-3-甲基-4-异丁酰基吡唑啉酮-5(PMIBP),1-苯基-3-甲基-4-特戊酰基吡唑啉酮-5(PMPVP),1-苯基-3-甲基-4-苯甲酰基吡 相似文献