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1.
紫外线吸收剂UV—326的合成 总被引:2,自引:0,他引:2
4-氯-2-硝基苯胺(1)用亚硝酸钠(2)和硫酸重氮化后与2-特丁基-4-甲基苯酚(3)反应制成2-硝基-4-氯-2′-羟基-3′-特丁基-5′-甲基偶氮苯(4)。其摩尔比为(1):(2):(3)=1:1.05:1.10,(4)用硫化钠还原制成2-(2′羟基-3′-特丁基-5′-甲基-)-5-氯苯并三唑N-氧化物(5),(5)用锌粉还原制成最终产品2-(2′-羟基-3′-特丁基-5′-甲基苯基)- 相似文献
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本工艺首先合成联苯乙酮,联苯甲酸乙酯,再从对-叔丁基苯基酰氯合成N-(4-叔丁基苯甲酰基)-N-(4′-联苯基酰基)-肼,然后完成2-(4′-叔丁基苯基)-5-(4′-联苯基)恶二唑-1,3,4(以下间称Bu-PBD)的合成。 相似文献
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研究了新合成的7种2-芳基-3-乙氧甲酰甲基-7-硝基-1,4-氧硫杂萘-4,4-二氧化物(AENBD)的电子轰击质谱,讨论了该类化合物的裂解规律。 相似文献
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本工作合成了新型的2-吡唑啉类化合物:1,3-二苯基-4-(p-硝基苄叉)-3-吡唑啉,研究了该化合物在室温及低温77K时的稳态光物理行为,结果表明:在标题化合物分子中存在着两种电荷转移机制,其一是从N1-N2-C3-苯基,基二是从N1-N2-C3-C4-P-硝基苄叉,光激发下,两种电荷转移机制相互竞争,且具有不同的发光构象。 相似文献
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新席夫碱萃取剂HPMαFP)2的合成及其在反相纸色谱中应用的研究 总被引:18,自引:0,他引:18
合成了新席夫碱萃取剂N,N'-A-双[(1-苯基-3-甲基-5氧-4-吡唑啉基)α-呋喃次基]乙二亚胺。通过元素分析、红外光谱、核磁共振谱、质谱和紫外光谱研究,了其结构及有关性质。 相似文献
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1,3,5-三芳基-2-吡唑啉化合物光物理行为的研究博士研究生闫正林导师吴世康(学位授予单位中国科学院感光化学研究所,北京100101)为了进一步了解电子转移过程中所存在的一些问题,本工作设计合成了一系列带不同取代基的1,3,5-三芳基-2-吡唑啉化... 相似文献
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A. Mustafa O. H. Hishmat M. M. Y. Younes 《Advanced Synthesis \u0026amp; Catalysis》1970,312(6):1011-1019
Both 4.6-dimethoxy-( 1c ) and 4.6.7-trimethoxy-5-acetoacetylbenzofuran 1d are obtained from visnaginone ( 1a ) and khellinone methyl ethers 1b , respectively, by a CLAISEN condensation. The β-diketones 1c and 1d couple with aromatic diazonium compounds to form the hydrazones 2a – i . 1-(4.6-Dimethoxybenzofuranyl)- and 1-(4.6.7-trimethoxybenzofuranyl)butane-1.2.3-trione-2-arylhydrazones 2 a–i react with hydrazine hydrate in acetic acid to yield the corresponding pyrazole derivatives 3a–i or 4a–i . The monohydrazones 5a–b are isolated when 2e or 2i are treated with hydrazine hydrate in ethanol. The hydrazones are converted to the respective pyrazoles by the action of glacial acetic acid. Hydroxylamine hydrochloride reacts with 1.2.3-trione-2-arylhydrazones 2a, c, e, f and i to yield the corresponding isoxazole derivatives 6a–e or 7a–e . The 2-arylhydrazones 2a, c, d, e, h and i form the corresponding pyrazole derivatives 8a–f when treated with semicarbazide hydrochloride. 相似文献
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Mosselhi A. N. Mosselhi Magda A. Abdallah Sayed M. Riyadh Abdelhamid E. Harhash Ahmad S. Shawali 《Advanced Synthesis \u0026amp; Catalysis》1998,340(2):160-164
The acid dissociation constants (Ka) of a series of 3,4-diaryl-1H-1,2,4-triazole-5-thiones ( 1 ) were determined and were found to correlated linearly with Hammett substituent constants; log Ka = 1.06 σx − 11.01. Such a result indicates that 1 exists essentially in one tautomeric form namely the thione form. Reactions of 1 with hydrazonoyl chlorides 2 gave the thiohydrazides 5 . Similiar reaction of 3-phenyl-1H(4H)- 1,2,4-triazole-5-thione 1g with 2a gave the thiohydrazide 5h which was converted into 1,3,5-triphenyl-1,2,4-triazolo[3,4-c]-1,2,4-triazole ( 9 ). The latter was also prepared from 3-phenyl-5-methylthio-4H-1,2,4-triazole ( 6 ) and 2a . The mechanism of the reaction of 1 with 2 is discussed. 相似文献
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Reactions of 3-arylhydrazones of 2,3,4-pentanetrione ( 1a–1e ) and 2-arylhydrazones of 1,3-diphenyl-1,2,3-propanetrione ( 1f–1l ) with 1,2-diaminoethane have been studied. It was found, that 3-arylhydrazones of 2,3,4-pentanetrione react with 1,2-diaminoethane with formation of 6-arylazo-2,3-dihydro-1,4-diazepines ( 2a–2e ) or the diarylazo derivatives of 4,9-dimethyl-5,8-diaza-3,9-dodecadiene-2,11-dione ( 3a–3e ). Analogous reactions of 2-arylhydrazones of 1,3-diphenyl-1,2,3-propanetrione yielded exclusively the derivatives of dihydrodiazepine. The structure of obtained products has been elucidated on the basis of i.r., m.s. and 1H-n.m.r. spectra. 相似文献
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The oxidation of naphthalene (1) (Scheme 1) in dichloromethane or acetonitrile with excess ozone gives phthalic aldehyde (3), 2-formyl benzoic acid (4) and phthalic anhydride (8). Small amounts of the (E)- and (Z)-isomer of 3-phenyl-(2-formyl)-propenal (10) and (11) are also observed in some cases. The reaction is faster in acetonitrile than in dichloromethane owing to the higher solubility of ozone in the former solvent. The reaction is faster on lowering the temperature because of the increase of the concentration of ozone in solution at lower temperature. With a 1:1 or a 1:2 naphthalene:ozone ratio high conversion and low selectivity for the anhydride (8) is observed. 相似文献
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Ali A. Abd-Elaal Ismail Aiad Samy M. Shaban Salah M. Tawfik Atef Sayed 《Journal of surfactants and detergents》2014,17(3):483-491
Three compounds namely; 5-(phenyl)-4H-1,2,4-triazole-3-thiol, 3-(decylthio)-5-phenyl-1H-1,2,4-triazole and 3-(benzylthio)-5-phenyl-1H-1,2,4-triazole) were synthesized. The chemical structure of the prepared compounds was confirmed using FTIR and 1H-NMR analysis. The compounds were tested as corrosion inhibitors against the corrosion of carbon steel in 1 M HCl using weight loss, polarization and electrochemical impedance methods. The results revealed that these compounds have significant inhibiting effects on the corrosion of carbon steel. Polarization studies showed that the compounds act as mixed-type inhibitors which retard the anodic and the cathodic reactions with a predominant effect towards the cathodic reaction. The prepared compounds were evaluated as antimicrobial agents against sulfate-reducing bacteria using the serial dilution method, which showed good biocidal action. 相似文献
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固体超强酸SO_4~(2-)/TiO_2催化合成利巴韦林缩合物研究 总被引:1,自引:0,他引:1
以1,2,4-三氮唑-3-羧酸甲酯和1,2,3,5-四-O-乙酰基-β-D-呋喃核糖为原料,在催化剂固体超强酸SO42-/TiO2的作用下得到了1-(2,3,5-三-O-乙酰基-β-D-呋喃核糖基)-1H-1,2,4-三唑-3-羧酸甲酯,简称利巴韦林缩合物。它是广谱抗病毒药物利巴韦林的重要中间体。通过对影响反应的多种因素进行研究以及反应条件的优化,结果表明:当催化剂为固体超强酸SO42-/TiO2、催化剂用量为12%、1,2,4-三氮唑-3-羧酸甲酯和1,2,3,5-四-O-乙酰基-β-D-呋喃核糖投料摩尔比为1.05:1、反应温度控制在100℃~110℃、反应时间为2h、甲醇重结晶,所得产物收率为87.0%,纯度99.5%(HPLC)。该反应方法催化剂易制备,催化效率较高,容易循环使用,不污染环境,有一定的再生能力,易从产品中除去,操作过程简便,产品色泽好、纯度高。 相似文献
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以1,4,5,6-四氢-6-哒嗪酮-3-甲酰肼和1,6-二氢-6-哒嗪酮-3-甲酰肼与1-苯基-3-芳基-4-甲酰基吡唑反应,得到相应的新化合物1,4,5,6-四氢-6-哒嗪酮-3-羰基吡唑醛腙和1,6-二氢-6-哒嗪酮-3-羰基吡唑醛腙.所有化合物的结构均经IR,1HNMR和元素分析得以证实. 相似文献
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Abdel Hamid Harhash Mohamed Hilmy Elnagdi Ebtisam Abdel Aziz Hafez 《Advanced Synthesis \u0026amp; Catalysis》1971,313(4):706-714
Treatment of 4-arylazo-2-alkoxy-2-thiazolin-5-ones 4a – f with glycine or phenylhydrazine effects their conversion into 1-aryl-5-alkoxy-1 H-1,2,4-triazole-3-carboxylic acid derivatives 5a – j , with the loss of hydrogen sulfide. On the other hand, the reaction of the 2-ethoxy ( 4a – c ) and the 2-isopropyloxy ( 4g – i ) derivatives with strong basic amines involves the loss of an alkyl mercaptan to yield the N-substituted amines 7d – j of 1-aryl-Δ2-1,2,4-triazolin-5-one-3-carboxylic acids. The 2-benzyloxy derivatives 4d – f react with the same reagents to give the N-substituted amides 2a – g of 1-aryl-Δ2-1,2,4-triazolin-5-thione-3-carboxylic acids, with the loss of benzyl alcohol. Hetero-ring opening of 4 , followed by recyclisation, occurs upon treatment with ethyl or phenyl magnesium halides to yield the triazolinethione derivatives 13 a – c . 相似文献
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Mostafa M. Ghorab Marwa G. El-Gazzar Mansour S. Alsaid 《International journal of molecular sciences》2014,15(5):7539-7553
4-Aminoantipyrine was utilized as key intermediate for the synthesis of pyrazolone derivatives bearing biologically active moieties. The newly synthesized compounds were characterized by IR, 1H- and 13C-NMR spectral and microanalytical studies. The compounds were screened as anticancer agents against a human tumor breast cancer cell line MCF7, and the results showed that (Z)-4-((3-amino-5-imino-1-phenyl-1H-pyrazol-4(5H)-ylidene)methylamino)-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 5, 3-(4-bromophenyl) -1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carbonitrile 13, 1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1-Hpyrazol- 4-yl)-3-(4-iodophenyl)-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carbonitrile 14, 3,3′-(4,4′-sulfonylbis(4,1-phenylene))bis(1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol- 4-yl)-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carbonitrile) 16, (Z)-1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-hydrazono-4-oxo-3-phenyl-1,2,3,4-tetrahydropyrimidine-5-carbonitrile 17, (Z)-1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-4-oxo-3-phenyl-2-(2-phenylhydrazono)-1,2,3,4-tetrahydro pyrimidine-5-carbonitrile 18, and (Z)-4-(3-amino-6-hydrazono-7-phenyl-6,7-dihydro pyrazolo[3,4-d]pyrimidin-5-yl)-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 19 were the most active compounds with IC50 values ranging from 30.68 to 60.72 μM compared with Doxorubicin as positive control with the IC50 value 71.8 μM. 相似文献
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《Journal of Sulfur Chemistry》2013,34(3):275-284
A series of some new fused thiopyrano[2,3-d]thiazole derivatives have been synthesized by a stereo-selective hetero-Diels-Alder reaction of 5-(2,4-dihydroxy-benzylidene)-4-thioxo-thiazolidine derivatives 3a,b with acrylonitrile, ethyl acrylate, N-phenylmale-imide, ω-nitrostyrene and N-phenyl-1, 3, 4-triazole-2,5-dione. 5-Amino-9-hydroxy-dihydro-benzopyrano[3′,4′:4,5]thiopyrano[2,3-d]thiazol-6-one derivatives 14a,b have been synthesized by Michael addition of 3a,b with malononitrile. Structures and conceivable mechanisms are discussed. 相似文献