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全氟3,4-二甲基-4-乙基-2-己烯(1)和含硫亲核试剂如苄硫酚、烯丙硫酚及苯硫酚等的反应及反应产物的转化可得四类异构体2,3,4,5;在-30~-60℃于乙醚中反应,得到动力学控制的产物2a~c。2a,2b与KF在DMF中,室温反应可转化为热力学稳定的产物3a,3b。在100~120℃,2a~c异构化为4a~c。后者在DMF-KF中室温反应,重排成5a~c。在DMF-NEt_3中2a再和苄硫酚反应得到连二苄硫醚(6)和含氢的端基烯7a及二取代产物8a,在乙醚-三乙胺中反应得到3a和9a。2a和甲醇反应,可得少量3a和10a。2b和二乙胺反应复杂,仅得少量3b和不饱和酰胺11。 相似文献
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2-(1H-1,2,4-三唑-1-基)-4,4-二甲基-1-烃硫基-3-戊酮的合成及波谱性质 总被引:2,自引:0,他引:2
由 2 - (1H - 1 ,2 ,4-三唑 - 1 -基 ) - 4 ,4-二甲基 - 1 -戊烯 - 3 -酮和硫酚 (醇 )亲核加成反应合成了五个未见文献报道的目标化合物 ,其化学结构经IR、1 HNMR、MS和元素分析确证并研究其波谱性质 相似文献
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(+)-1S,2R,5S-8-β萘基薄荷醇的合成 总被引:3,自引:0,他引:3
以R-(+)-Pulegone为起始原料经1,4-加成、溴代、水解、氧化等9步反应合成了手性辅助试剂(+)-1S,2R,5S-8-β-萘基薄荷醇及其差向异构体(一)-1R,2R,5S-8-β-萘基新薄荷醇,总收率分别为24.0%和22.6%. 相似文献
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α-(1H-1,2,4-三唑-1-基)-β-芳硫基取代苯酮的合成及生物活性研究 总被引:1,自引:0,他引:1
利用 2 (1H 1,2 ,4 三唑 1 基 ) 2 丙烯 1 酮 (2 )与取代硫酚或含巯基的杂环化合物进行 1,4 亲核加成 ,得到目标化合物 3,其结构经元素分析、核磁和红外光谱所证实 ,并对其进行了生物活性的测试 ,发现大部分化合物具有很好的抑菌活性 .结构与活性的关系表明不同的R1取代对其生物活性有较大的影响 ,当R1=(CH3 ) 3 C时 ,对小麦锈病的抑制活性要高于R1=Ar的活性 ,而Ar上不同的取代基对其活性影响不大 相似文献
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全氟3,4-二甲基-4-乙基-2-己烯(1)和含硫亲核试剂如苄硫酚、烯丙硫酚及苯硫酚等的反应及反应产物的转化可得四类异构体2,3,4,5;在-30~-60℃于乙醚中反应,得到动力学控制的产物2a~c.2a,2b与KF在DMF中,室温反应可转化为热力学稳定的产物3a,3b,在100~120℃,2a~c异构化为4a~c.后者在DMF-KF中室温反应,重排成5a~c.在DMF-NEt3中2a再和苄硫粉反应得到连二苄硫醚(6)和含氢的端基烯7a及二取代产物8a,在乙醚-三乙胺中反应得到3a和9a,2a和甲醇反应,可得少量3a和10a,2b和二乙胺反应复杂,仅得少量3b和不饱和酰胺11。 相似文献
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α-(1H-1,2,4-三唑-1-基)-β-芳硫基取代苯酮的合成及生物活性研究 总被引:2,自引:0,他引:2
利用2-(1H-1,2,4-三唑-1-基)-2-丙烯-1-酮(2)与取代硫酚或含巯基的 杂环化合物进行1,4-亲核加成,得到目标化合物3,其结构经元素分析、核磁和红 外光谱所证实,并对其进行了生物活性的测试,发现大部分化合物具有很好的抑菌 活性。结构与活性的关系表明不同的R~1取代对其生物活性有较大的影响,当R~1 = (CH_3)_3C时,对小麦锈病的抑制活性要高于R~1 = Ar的活性,而Ar上不同的 取代基对其活性影响不大。 相似文献
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Tetrachloro-1, 2-benzoquinone and 2, 3-dichloro-1, 4-naphthoquinone react with a series of aryl and alkyl selenolate, generated either by the reaction of Grignard reagents and selenium powder or by the reduction of diselenides with NaBH4, to give 3, 6-diarylseleno-2, 5-dichloro-1, 4-benzoquinones 3 and 2, 3-diarylseleno-1, 4-naphthoquinones 4 in good yields. 相似文献
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A series of novel 2,6-diaryl-3-(arylthio)piperidin-4-ones have been synthesized by reaction of arylthioacetones, substituted aromatic aldehydes, and methylamine/ammonium acetate and their structures elucidated by (1)H, (13)C, and 2D NMR (H, H-COSY, C, H-COSY, HMBC, and NOESY) spectroscopy. The NMR data reveal that all these piperidones exist in chair conformation with the 2,6-diaryl groups equatorially oriented, while the arylthio group prefers to be in either an equatorial or axial orientation depending on whether the substituent in the 2,6-diaryl rings is present in 4- or 2-position, respectively. In the case of NH-2,6-diaryl-3-(arylthio)piperidin-4-ones with o-substituted 2,6-diaryl groups, the arylthio group prefers the axial orientation presumably in a bid to minimize the steric and/or electronic repulsion. The arylthiopiperidin-4-ones exhibit significant antibacterial activity against Staphylococcus aureus, Vibrio cholerae, Salmonella typhi, and Escherichia coli and antifungal activity against Candida albicans and Aspergillus niger. 相似文献
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Asymmetric 3,5-diaryl substituted 4H-1,2,6-thiadiazin-4-ones can be prepared from 3,5-dichloro-4H-1,2,6-thiadiazin-4-one (1) via a multi-step protocol: selective nucleophilic mono-chloro substitution gives either the mono-methoxy or benzyloxy substituted mono-chlorothiadiazinones that can be phenylated via Suzuki–Miyaura coupling. Subsequent BBr3 mediated dealkylation gives 3-hydroxy-5-phenyl-4H-1,2,6-thiadiazin-4-one (9) that can be activated by a modified Finkelstein halodehydroxylation via the triflate, enabling further arylation reactions using Suzuki–Miyaura or Stille coupling chemistry. 相似文献
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研究了3-(2'-苯基-1', 2', 3'-连三唑-4'-基)-4-氨基-5-巯基-1, 2, 4-三唑(1)与取代苯甲酸和脂肪酸(2a-r)在POCl3催化下的反应, 共合成得到18个新的3-(2'-苯基-1', 2', 3'-连三唑-4'-基)-6-烷基/芳基-均三唑并[3, 4-b]-1, 3, 4-噻二唑(3a-r), 经元素分析,IR, 1H NMR和MS进行了结构确证。 相似文献
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Jian Ge ZHANG Chang Sheng JIANG Guo Qiang LIN Ren WEN 《中国化学快报》2005,16(9):1205-1208
A new method for the synthesis of 4, 4-diaryl/diheteroaryl-3-butenyl derivatives of nipecotic acid as GABA transporter inhibitors is described. The key intermediates 4-tosyl-1, 1-diaryl/diheteroaryl-1-butene 10a-d were synthesized by Wittig reaction, and followed by alkylation with (R)-3-piperidinecarboxylate. The resulting N-cycloalkylated amino acid esters 11a-d were saponified and then acidified to get the target compounds 1a-d. The preliminary bioassays showed that la-d exhibited excellent inhibition of [3H]-GABA uptake in vitro of culture cells. 相似文献
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[reaction: see text] The first direct reductive amination of mucochloric acid (1) has been accomplished. Reaction of 1 with various alkyl, aryl, and benzylamines, followed by reduction in the same pot, provides an efficient method of obtaining N-benzyl-3,4-dichloro-1,5-dihydro-pyrrol-2-one and N-aryl (or alkyl)-3,4-dichloro-1,5-dihydro-pyrrol-2-ones. 相似文献
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The condensation reaction between 5-amino-4,6-dichloro-2-methylprimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4,6-dichloro-2-methyl-5-(1-acetyl-tetra-hydro-imidazo-2-ylidene)-aminopyrimidine predominantly and 4,6-dichloro-2-methyl-5-{1-1-(2-oxo-tetrahydro-imidazolyl)]-acetene}-aminopyrimidine as by-product. No 4,6-dichloro-2-methyl-5-(1-acetyl-2-imidazolin-2-yl)-aminopyrimidine was found. The result indicated an esterifi-cation-addition-elimination mechanism. 相似文献
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The reaction of 1-substituted-3-methylpyrazol-5-ones 1 with alkyl chloroformates and calcium hydroxide in dioxane have been studied. With 1-phenyl-3-methylpyrazol-5-one, the isolated product was alkyl 3-methyl-5-oxo-1-phenylpyrazole-4-carboxylate 2 but with 1-alkyl-3-methylpyrazol-5-one formation of 1-alkyl-5-alkoxycarbonyloxy-3-methylpyrazole 3 was observed. Replacement of alkyl chloroformate by bis(alkoxythiocarbonyl) sulfide results in the formation of 4-alkoxythiocarbonyl derivatives 4 in low yield with both 1-substituted-3-methylpyrazol-5-ones. 相似文献
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Iranpoor N Firouzabadi H Akhlaghinia B Nowrouzi N 《The Journal of organic chemistry》2004,69(7):2562-2564
Triphenylphosphine and 2,3-dichloro-5,6-dicyanobenzoquinone afford an adduct, which in the presence of n-Bu(4)NCN converts alcohols, thiols, and trimethylsilyl ethers into their corresponding alkyl cyanides in good to excellent yields at room temperature. This method is highly selective for the conversion of 1 degrees alcohols in the presence of 2 degrees and 3 degrees ones, thiols and silyl ethers. 相似文献
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Vishnu J. Ram Vidyottama Dube Luc A. C. Pieters Arnold J. Vlietinck 《Journal of heterocyclic chemistry》1989,26(3):625-628
Various bis[4-aryl/alkyl-1, 2, 4-triazoline-5-thione-3-yl]alkanes ( 3 ) were prepared from base cyclization of bis thiosemicarbazide 2 and transformed into sulphides by reaction with different alkyl halides in alkaline medium. These compounds were further oxidised to sulphones 5 with acidic potassium permanganate. 1-Aryl-3-[4-(4-aryl/alkyl-1, 2, 4-triazoline-3-thione-5-yl)phenyl]thioureas ( 8 ) were prepared in two steps from p-aminophenylhydrazide ( 6 ) and aryl/alkylisothiocyanates. Alkylation of 8 with different alkyl halides yielded exclusively sulphides 9 . Some sulphides 12 and Mannich bases 13 from 5-(p-fluorophenyl)-1, 3, 4-oxadiazol-2-thione ( 11 ) were also prepared to evaluate their pesticidal activities. All the prepared compounds were screened for pesticidal activities but none of them exhibited any significant activity. 相似文献