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1.
1,3,4,6—四硫代戊搭烯—2,5—二酮制备含硫取代基的四硫富瓦… 总被引:3,自引:0,他引:3
以1,3,4,6-四硫代戊搭烯-2,5-二酮为原料,经偶联,醇解,烃化或醇解,烃化,偶联等步骤,制得四甲硫基四硫富瓦烯,四乙硫基四硫富瓦烃,二喹喔啉硫醚,4-甲硫基-5-甲氧甲酰硫基-1,3-二硫环戊烯-2-酮。四甲基乙烯和4,4'-二甲硫基-5,5'-二甲氧甲酰硫基四硫富瓦烯及它的异构体混合物,提出了1,3,4,6-四硫代戊搭烯-2,5-二酮醇解机理。讨论了未得到某些预期产物的原因,报道了3种四 相似文献
2.
烷硫基甲硫富瓦烯的合成及其性质的研究 总被引:1,自引:0,他引:1
分别以1,3,4,6-四硫代戊搭烯-2,5-二酮和4,5-二(2′-氰基乙硫基)-1,3-二硫杂环戊烯-2-酮为原料,经偶联、醇解、烃化制得四甲硫基甲硫富瓦烯和四乙硫基四硫富瓦烯。对两种方法制得产物的产率存在较大差别提出了合理的解释,并讨论了2种四硫富瓦烯衍生物的循环伏安图及有关电化学性质。 相似文献
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以二(1,3-二硫杂环戊烯-2-硫酮-4,5-二硫)合锌酸四乙基铵为基原料,经苯甲酰化,醇解,苄基化,偶联,得到5个未见文献报道的四苄硫基四硫富瓦烯衍生物,报道了它们的循环伏安图及UV-Vis吸收光谱,对其电化学性质的变化规律做出了合理的解释。 相似文献
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TTF·M(dmit)2型电荷转移配合物的合成及其拉曼光谱 总被引:2,自引:0,他引:2
合成了8种四硫富瓦烯·二-(1,3-二硫杂环戊-4-烯-2-硫酮-4,5-二巯基)金属(缩写为TTF·M(dmit)-2)电荷转移配合物,其中7种配合物为首次合成,拉曼光谱的研究结果表明,对同一种电子受体,电子给体的还原电势Ep越小,配合物的电荷转移度ρ值越大。 相似文献
7.
双(6,7-二甲硫基四硫富瓦烯-2,3-二硫)金属配合物的合成 总被引:5,自引:0,他引:5
以6,7-二甲硫基四硫富瓦烯-2,3-二硫盐为配体合成了3种未见文献报道的双(6,7-二甲硫基四硫富瓦烯-2,3-二硫)金属配合物,为“桥式”四硫富瓦烯衍生物的合成创造出一种新方法,并对只得到中性产物提出了合理的解释。研究了其IR及室温电导率。 相似文献
8.
报道了N-烷基5-甲酰胺基-1,2,4-氧杂二唑基-3-β-D-吡喃木糖用二乙胺基三氟化硫选择性氟化,得到相应的N-烷基-5-甲酰胺基-1,2,4-氧杂二唑基-3-(4'-脱氧-4'-氟-β-L-吡喃型阿拉伯糖);并用光谱分析确证了它们的构型及在溶液中的构象。 相似文献
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2,6-二(甲硫基)-3,7-二(2-氰乙基硫基)四硫富瓦烯在甲醇钠的作用下消除保护基团, 生成四硫富瓦烯双钠盐, 再与9,10-二(氯甲基)蒽反应生成由四硫富瓦烯(TTF)和蒽单元构建的新型TTF环蕃. 分别通过循环伏安法和化学氧化法对其电化学性质、紫外吸收光谱和荧光性质进行了研究, 实验结果表明此类TTF环蕃化合物对OH-离子有识别功能. 并通过电化学和紫外吸收光谱研究了这种新型四硫富瓦烯环蕃在金纳米颗粒表面自组装行为. 相似文献
11.
Cheng MF Yu HM Ko BW Chang Y Chen MY Ho TI Tsai YM Fang JM 《Organic & biomolecular chemistry》2006,4(3):510-518
The expedient synthesis of various 1,4-benzodiazepine-2,5-dione compounds, particularly those having substituents at the C3-, N1- and N4-positions is achieved. The important features in these synthetic strategies include: (i) using the coupling reaction of isatoic anhydride with alpha-amino ester for direct construction of the core structure of 1,4-benzodiazepine-2,5-dione; (ii) using potassium carbonate as the base of choice for selective alkylation at the N1-site, while using lithiated 2-ethylacetanilide as the required base to furnish the N4-alkylation; and (iii) using 2-nitrobenzoyl chloride as a synthetic equivalent of anthranilic acid to facilitate the polyethylene resin-bound liquid-phase combinatorial synthesis. The prepared 1,4-benzodiazepine-2,5-dione compounds are evaluated for endothelin receptor antagonism by a functional assay that measures the inhibitory activity against the change of intramolecular calcium ion concentration induced by endothelin-1. The preliminary results indicate that 1,4-benzodiazepine-2,5-diones bearing two flanked aryl substituents at the N1- and N4-sites show better inhibitory activity than the corresponding unalkylated and N-monoalkylated compounds. A promising candidate, 1-benzyl-7-chloro-3-isopropyl-4-(3-methoxybenzyl)-1,4-benzodiazepine-2,5-dione (17b), exhibits an IC50 value in low nM range. 相似文献
12.
Ouyang J Yakushi K Kinoshita T Nanbu N Aoyagi M Misaki Y Tanaka K 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2002,58(8):1643-1656
Infrared and Raman spectra of 2,5-bis(1,3-dithiol-2-ylidene)-1,3,4,6-tetrathiapentalene (BDT-TTP) and 1,3,4,6-tetrathiapentalene-2,5-dione (TTP-DO) are reported. The vibrational modes of TTP-DO are assigned with the aid of the depolarization ratio of solution Raman spectra, polarized reflection spectra and polarized Raman spectra. A D2h symmetry is assumed for the BDT-TTP molecule and its in-plane fundamental vibrations are assigned with the aid of the polarization ratio and the correlation with TTP-DO, tetrathiafulvalene (TTF), tetramethyltetrathiafulvalene (TMTTF) and bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF). Normal coordinate calculation with a modified internal valence force field was carried out for the in-plane fundamental vibrations of TTP-DO and BDT-TTP. Ab initio calculations of the normal modes of BDT-TTP0 and BDT-TTP+ are compared with the empirical analysis. 相似文献
13.
Arthur F. Lewis Ganapathi R. Revankar Susan M. Fennewald Robert F. Rando John H. Huffman 《Journal of heterocyclic chemistry》1995,32(2):547-556
Alkyl derivatives of the thiazolo[4,5-d]pyrimidine congeners of guanine and uracil were prepared and assessed for in vitro activity against human cytomegalovirus (HCMV). The finding that the 3-pentyl 1b and 3-hexyl 1c derivatives of 5-aminothiazolo[4,5-d]pyrimidine-2,7(3H,6H)-dione (1e) had potent in vitro anti-HCMV activity prompted a broader study of alkyl derivatives in this ring system. A series of 3-alkyl derivatives of 1e , viz. 1f-w , were prepared by direct alkylation of the sodium salt of 1e and by subsequent modifications, 2a-d. For comparison with 1c , 5-amino-2-hexylaminothiazolo[4,5-d]pyrimidin-7(6H)-one (4) was prepared and studied. The 3-(2-alkenyl) derivatives of 1e were found to be the more active antiviral agents with the Z isomer of 5-amino-3-(2-penten-1-yl)thiazolo[4,5-d]pyrimidine-2,7(3H,6H)-dione (1f) having the better therapeutic index. Analogous 4-(2-alkenyl) derivatives of 2-aminothiazolo[4,5-d]pyrimidine-5,7(4H,6H)-dione 6a and 6b were also prepared but were found to have poor therapeutic indices. Single crystal X-ray diffraction analysis was used to unequivocally establish the structure of 1f. 相似文献
14.
Harald Müller Anna Puig Molina B. Zh. Narymbetov L. V. Zorina S. S. Khasanov R. P. Shibaeva 《无机化学与普通化学杂志》1998,624(9):1492-1496
The title compounds were prepared from 1,3,4,6-tetrathiapentalene-2,5-dione ( 1 ) in one step via the in situ generated intermediate 2-oxo-1,3-dithiole-4,5-dithiolate (dmid; 2 ). The X-ray single crystal structure of (Et4N)2[Zn(dmid)2] ( 3 a ) gave the tetragonal space group P43212 with a = b = 13.810(2) Å, c = 16.480(3) Å, and Z = 4. (n-Bu4N)2[Zn(dmid)2] ( 3 b ) gave the triclinic space group P 1 with a = 11.947(4) Å, b = 14.665(5) Å, c = 16.662(8) Å, α = 100.21(3)°, β = 104.46(3)°, γ = 110.73(3)°, and Z = 2. 相似文献
15.
Toshio Tanaka Noriaki Okamura Kiyoshi Bannai Atsuo Hazato Satoshi Sugiura Koji Tomimori Kenji Manabe Seizi Kurozumi 《Tetrahedron》1986,42(24):6747-6758
(5
)-Prostaglandin E2 (7) was synthesized fron (
)-4-
-butyldimethylsilyloxy-2-cyclopentenone (1) by
2-alkenyloxycarbonylatlon of the organocopper conjugate-addition adduct (3) followed by intramolecular palladium-catalyzed decarboxylative allylic alkylation. The (5
)-prostaglandin E2 skeleton was also obtained from the β-keto allylic ester (11) by a similar decarboxylative allylic alkylation. The decarboxylative allylic alkylation of another type of the three-component coupling product (12) gave new 6-methyleneprostaglandin E1 skeleton (15a), which was converted into new 6-methylprosta-glandin I methyl ester (20)
6-methyleneprostaglandin F1 derivative (16) by two different ways. The stereochemistry of this intramolecular decarboxylative allylic alkylation was discussed in the reaction of 2-[(
)- or (
)-2-butenyloxy-carbonyl] cyclopentanone systems. 相似文献
16.
在乙酰乙酸乙酯和氧化亚铜共同催化下, 二-(1,3-二硫环戊烯-2-硫酮-4,5-二硫)合锌酸四乙基铵盐分别与2-碘吡啶(1a)、 3-碘吡啶(1b)和4-碘吡啶(1c)反应, 制得硫酮化合物2,3-二(2-吡啶硫基)-1,3-二硫环戊烯-2-硫酮(2a)、 2,3-二(3-吡啶硫基)-1,3-二硫环戊烯-2-硫酮(2b)和2,3-二(4-吡啶硫基)-1,3-二硫环戊烯-2-硫酮(2c). 在醋酸汞催化下, 硫酮化合物2a, 2b和2c分别被氧化为2,3-二(2-吡啶硫基)-1,3-二硫环戊烯-2-酮(3a)、 2,3-二(3-吡啶硫基)-1,3-二硫环戊烯-2-酮(3b)和2,3-二(4-吡啶硫基)-1,3-二硫环戊烯-2-酮(3c). 以亚磷酸三乙酯为偶联剂, 氧酮化合物3a, 3b和3c分别发生自偶联反应生成2,3,6,7-四(2-吡啶硫基)四硫富瓦烯(4a)、 2,3,6,7-四(3-吡啶硫基)四硫富瓦烯(4b)和2,3,6,7-四(4-吡啶硫基)四硫富瓦烯(4c). 采用核磁共振波谱(NMR)、 傅里叶变换红外光谱(FTIR)和质谱(MS)分析了所合成化合物的结构和组成, 通过X射线衍射分析确认了吡啶基四硫富瓦烯衍生物4b和4c的晶体结构. 循环伏安法研究结果表明, 化合物4a, 4b和4c呈现准可逆的两电子转移过程, 结合量子化学计算, 分析了不同位置取代的吡啶基对四硫富瓦烯电化学电势的影响. 相似文献
17.
《Tetrahedron: Asymmetry》1998,9(15):2635-2639
An efficient enantioselective synthesis of the title compound I was developed from the versatile chiron 1-tert-butyldimethylsilylpenta-1,4-diyn-3-ol 2. The chiron, in turn, was prepared via a combination of lipase catalyzed acylation–alcoholysis protocol. Protection of its hydroxy group, alkylation with a suitable bromide and subsequent functionalization gave (S)-I with high enantiomeric purity. 相似文献
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V. A. Kataev S. A. Meshcheryakova V. V. Lazarev V. V. Kuznetsov 《Russian Journal of Organic Chemistry》2013,49(5):743-745
Reactions of 6-methylpyrimidine-2,4(1H,3H)-dione or 5-hydroxy-6-methyl-pyrimidine-2,4(1H,3H)-dione with 2-chloromethylthiirane afforded the corresponding substituted 1-(thietan-3-yl)pyrimidine-2,4(1H,3H)-diones. The calculations in the framework of approximations PBE/3z, B3LYP/6-31G++(d,p) and MP2/6-31G++(d,p) showed that the alkylation occurred at the atom N1 of the pyrimidine ring. 相似文献
20.
Liu C Wang X Pei T Widenhoefer RA 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(24):6343-6352
Reaction of 8-nonene-2,4-dione with a catalytic amount of [PdCl2(CH3CN)2] (2; 5 mol %) and a stoichiometric amount of CuCl2 (2.5 equiv) at room temperature for 3 h led to oxidative alkylation and formation of 2-acetyl-3-methyl-2-cyclohexenone in 80 % isolated yield. The oxidative alkylation of 4-pentenyl beta-diketones tolerated a number of terminal acyl groups and substitution at the C1 and C3 carbon atoms of the 4-pentenyl chain. Likewise, 4-pentenyl beta-keto esters that possessed geminal disubstitution at the C1, C2, or C3 carbon atom of the 4-pentenyl chain cyclized to form 2-carboalkoxy-2-cyclohexenones in moderate to good yield as the exclusive cyclized product. Deuterium-labeling experiments provided information regarding the mechanism of the palladium-catalyzed oxidative alkylation of 4-pentenyl beta-dicarbonyl compounds. 相似文献