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1.
在阳离子交换树脂D72存在下5-氨基-3-苄硫基-4-氰基(乙氧羰基)吡唑与苯基二氯化膦和芳醛的类Mannich反应,合成了9个2-苄硫基-3-氰基(乙氧羰基)-5-芳基-6-苯基-6-氧-6-磷杂-4,5,6-三氢咪唑[2,3e]吡唑,利用NMR方法确定其为反式构型,初步研究了反应机制。生物活性测试结果表明,部分化合物具有一定的除草活性。 相似文献
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吡唑类衍生物是一类具有很好生物活性的化合物,具有很高除草或杀虫活性的吡唑类化合物文献中已有大量的报导[1]。因此研究其合成方法显得很重要。我们最初希望通过5-氨基-3-苄硫基-4-乙氧羰基吡唑经重氮化反应去氨基制备3-苄硫基-4-乙氧羰基吡唑,然后继续衍生化合成系列吡唑类化合物。 相似文献
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根据活性亚结构拼接原理,将3-芳基-4-氨基-5-乙氧羰基(氰基)-3H-噻唑啉-2-硫酮与酰氯反应得到目标化合物3-芳基-4-取代苯氧乙酰氨基-5-乙氧羰基(氰基)-3H-噻唑啉-2-硫酮.再以3-苯基-4-氨基-5-乙氧羰基-3H-噻唑啉-2-硫酮为合成原料,经过Aza-Wittig反应得到目标化合物5-芳氧基-3,6-二芳基-2-硫代噻唑并[4,5-d]嘧啶-7-酮.通过IR,1H NMR,EI-MS,元素分析等方法对所合成的化合物进行了结构表征.代表化合物5-对氯苯氧基-3,6-二苯基-2-硫代-2,3-二氢噻唑并[4,5-d]嘧啶-7(6H)-酮(C1)经单晶X衍射证实了结构.除草活性测试结果表明:部分噻唑啉-2-酮类衍生物对稗草和油菜都表现出了较好的抑制活性. 相似文献
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为了寻求新的N-芳基吡唑类先导化合物, 用5种拟除虫菊酯类农药的活性基团——菊酸与高活性杀虫剂氟虫腈和其中间体5-氨基-3-氰基-1-(2,6-二氯-4-三氟甲基-苯基)吡唑在其氨基位置采用亚结构对接的方法合成得到了10个新的芳基吡唑菊酰胺类化合物. 经1H NMR, ESI-MS和元素分析对化合物的结构进行了表征. 初步生物活性测定结果表明, 在37.5 mg/L浓度下, N-[3-氰基-1-(2,6-二氯-4-三氟甲基苯基)-4-(三氟甲基亚磺酰基)-1H-吡咯-5-基]-3-(2,2-二氯乙烯基)-2,2-二甲基环丙酰胺(3b)对小菜蛾Amaranthus spinosus抑制活性达到100%, LC50为15.1 mg/L. 初步雌雄大鼠急性经口毒性综合评价属中毒级, 同时还检测了2-(4-氯苯基)-N-[3-氰基-1-(2,6-二氯-4-三氟甲基苯基)-1H-吡唑-5-基]-3-甲基丁酰胺(3i)的晶体结构. 相似文献
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Salvatore Plescia Giuseppe Daidone Maria L. Bajardi 《Journal of heterocyclic chemistry》1982,19(3):685-687
By reaction of some 4-carbethoxy(or cyano)-3(5)-R-5(3)-aminopyrazoles 1 with 2-nitrobenzoyl chloride or 2-nitrobenzenesulfonyl chloride, a number of novel 3- and 5-amino-1-(2-nitrobenzoyl or 2-nitrobenzene-sulfonyl)pyrazoles 6 and 7 were obtained. Every compound appearing during the endocyclic N-substitution process can be identified and determined by glc. The use of nmr offers a rapid, unambigous method for determining the proposed structures. 相似文献
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Katritzky AR Akhmedov NG Abdel-Fattah AA Wang M Rostek CJ Maender OW 《Magnetic resonance in chemistry : MRC》2004,42(5):424-435
Nucleophilic addition of alkyl- and benzylthiols to benzoquinone diimine (1) gave the corresponding 3-alkylthio- or 3-benzylthio-1,4-phenylenediamines (2-5). However, addition of aryl- or heteroarylthiols to 1 formed 2-arylthio- or 2-heteroarylthio-1,4-phenylenediamines (6-14). The structures of 2-14, obtained in 55-91% yields, were confirmed in CDCl3 or DMSO-d6 solution using 1D (NOE difference, coupled 13C NMR spectra, APT and DEPT) and 2D NMR techniques [DQCOSY, NOESY, HETCOR and heteronuclear multiple bond coherence (HMBC)] that resulted in unambiguous proton and carbon NMR resonance assignments. The substituent-induced 13C NMR chemical shift differences were calculated in 2-14 relative to carbon atoms in the model compound N1-(1,3-dimethylbutyl)-N4-phenyl-1,4-phenylenediamine (DMBPPD) (15) (a reduced form of benzoquinone diimine). 相似文献
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This work presents the substituent effects on the 1H and 13C NMR chemical shifts in the cis-isomer of 3-Y-cyclohexanols (Y = Cl, Br, I, CH3, N(CH3)2 and OCH3) and 3-Y-1-methoxycyclohexanes (Y = F, Cl, Br, I, CH3, N(CH3)2 and OCH3). It was observed that the H-3 chemical shift, due to the substituent alpha-effect, increases with the increase of substituent electronegativity when Y is from the second row of the periodic table of elements, (CH3 *sigma(C3--H3a) interaction energy. This interaction energy, for the halogenated compounds, decreases with an increase in size of the halogen, and this is a possible reason for the largest measured chemical shift for H-3 of the iodo-derivatives. The beta-effect of the analyzed compounds showed that the chemical shift of hydrogens at C-2 and C-4 increases with the decrease of n(Y) --> *sigma(C2-C3) and n(Y) --> *sigma(C3-C4) interaction energies, respectively, showing a behavior similar to H-3. The alpha-effect on 13C chemical shifts correlates well with substituent electronegativity, while the beta-effect is inversely related to electronegativity in halogenated compounds. NBO analysis indicated that the substituent inductive effect is the predominant effect on 13C NMR chemical shift changes for the alpha-carbon. It was also observed that C-2 and C-4 chemical shifts for compounds with N(CH3)2, OCH3 and F are more shielded in comparison to the compounds having a halogen, most probably because of the larger interaction of the lone pair of more electronegative atoms (n(N) > n(O) > n(F)) with *sigma(C2-C3), *sigma(C3-C4) and *sigma(C3-H3a) in comparison with the same type of interaction with the lone pair of the other halogens. 相似文献
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Certain 5-aryl-6-[tetra(O-benzoyl)-β-D-glucopyranosylimino]-4-benzylthio-2-phenylimino-5,6-dihydro-2H-1,3,5-thiadiazines have
been prepared by interaction of N-[tetra(O-benzoyl)-β-D-glucopyranosyl] isocyanodichloride and 1-aryl-5-phenyl-2-(S-benzyl)-2,4-isodithiobiurets.
The products have been characterized through the usual chemical transformations, IR, NMR and mass spectral analyses. The compounds
have been screened for their antibacterial activities against various bacteria.
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Published in Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 910–913, June, 2005. 相似文献
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Parthiban P Balasubramanian S Aridoss G Kabilan S 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2008,70(1):11-24
Variously substituted 2,6-diarylpiperidin-4-one O-benzyloximes were synthesized by the direct condensation of the corresponding 2,6-diarylpiperidin-4-ones with O-benzylhydroxylamine hydrochloride. All the synthesized compounds are characterized by IR, Mass and NMR spectral studies. NMR spectral assignments are made unambiguously by their one-dimensional (1H NMR and 13C NMR) and two-dimensional (1H-1H COSY, NOESY, HSQC and HMBC) NMR spectra. All the synthesized compounds are resulted as single isomer, i.e., exclusively E isomer (9-14). The conformational preference of 2,6-diarylpiperidin-4-one oxime ethers with and without alkyl substituents at C-3 and C-5 has also been discussed using the spectral studies. The observed chemical shifts and coupling constants suggest that compounds 8-13 adopt normal chair conformation with equatorial orientation of all the substituents while compound 14 contributes significant boat conformation along with the predominant chair conformation in solution. The effect of oximination on ring carbons, their associated protons, alkyl substituents and ipso carbons are studied. Every proton in the piperidone ring of the oxime ether is observed as distinct signal due to oximination. The order of chemical shift magnitude in compound 8 is H-2a>H-6a>H-5e>H-3e>H-3a>H-5a. For 9-12, the order is H-6a>H-5e>H-2a>H-3a>H-5a, for 13, H-6a>H-2a>H-5e>H-3a>H-5a and for 14, the order is H-2a>H-6a>H-5e>H-3a>H-5a while the 13C chemical shift magnitude for 8-14 due to oximination is C-2>C-6>C-3>C-5. 相似文献
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The reaction with hydrazine of 4-carbethoxy or acetyl 5-methyl(2H)furanones 2-substituted by arylmethine, alkenylmethine, arylaminomethine produces new 4,5-dihydro 3-methyl 4-oxo pyrazolo(3,4d)pyridazines or 3,4-dimethyl pyrazolo(3,4d)pyridazines. The preparation of 3-arylacetyl 4-carbethoxy or acetyl 5-methyl pyrazoles is described. 相似文献
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Five 5-substituted-4-(arylidene)amino-2,4-dihydro-3H-1, 2,4-triazole-3-thiones (2a-2e) and seven 6-aryl-3-(D-gluco-pentitol-1-yl)-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazines (3a-3g) were synthesized. The complete 1H and 13C NMR chemical shift assignments were analyzed on one- and two-dimensional NMR techniques, including DEPT, NOE-DIF, COSY, gHMBC, and gHSQC. 相似文献
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A. D. Dyachenko S. M. Desenko V. D. Dyachenko A. N. Chernega 《Chemistry of Heterocyclic Compounds》2004,40(8):1009-1016
The condensation of cyclohexylidenemalononitrile or cyclohexylidenecyanoacetic ester with thioamidoethyl(methyl)malonate in the presence of sodium ethylate gave 6-amino-3-carbethoxy-5-cyano-4-spirocyclohexane-1,2,3,4-tetrahydropyridine-2-thione and 3-carbethoxy(methoxy)-5-cyano-6-oxo-4-spirocyclohexanepiperidine-2-thiones which were used in the synthesis of the corresponding substituted 2-alkylthiotetrahydropyridines. 5-Carbethoxy-3-cyano-3-methyl-6-methylthio-4-spiro-cyclohexane-3,4-dihydropyridine-2(1H)-one was studied by X-ray crystallography. 相似文献
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The orientation of the addition of 5-amino-3-benzylthio-1,2,4-triazole and its analogues (pyrazole) (1) with the aryl isocyanate can be directed by controlling the reaction temperature and one of the product, 5-amino-1-arylaminocarbonyl-3-benzylthio-1,2,4-triazole (pyrazole) (2), can rearrange at 170°C to another product, 5-arylureylene-3-benzylthio-1,2,4-triazole (pyrazole) (3). A plausible mechanism explanation for this rearrangement reaction was presented. It was suggested that the rearrangement reaction could be referred to the thermodynamics transposition leading to the predominant 5-arylureylene-3-benzylthio-1,2,4-triazole energy preferentially. 相似文献
20.
Burgeson JR Renner MK Hardt I Ferrence GM Standard JM Hitchcock SR 《The Journal of organic chemistry》2004,69(3):727-734
Asymmetric aldol reactions were conducted with the titanium enolate of N(3)-hydrocinnamoyl-3,4,5,6-tetrahydro-2H-1,3,4-oxadiazin-2-one to afford aldol adducts 5a-j. The dominant product of the asymmetric aldol reaction was the non-Evans syn adduct as determined by (1)H NMR spectroscopy and X-ray crystallography. When evaluating the (1)H NMR spectra of adducts 5a-j, a highly shielded signal with an average chemical shift of 0.05 ppm was observed. This signal was readily determined to be the C(5)-methyl group of the oxadiazinone. It is presumed that the overall conformation adopted by the aldol adducts in solution places an aromatic ring of the N(3)-substituent in close proximity to the C(5)-methyl group. An investigation of this conformational preference is conducted employing (1)H NMR spectroscopy, X-ray crystallography, and computational methods. 相似文献