共查询到18条相似文献,搜索用时 93 毫秒
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以三聚氯氰(1)和γ-氨丙基三乙氧基硅烷(2)为原料,经亲核取代反应合成了一种新型三嗪类氮-硅成炭剂——2-氯-4,6-二(3-三乙氧基硅烷基-1-氨丙基)-1,3,5-三嗪(3),其结构和热性能经1H NMR,IR和TGA表征。考察了溶剂、缚酸剂、原料比和反应温度对3产率的影响。合成3的最佳反应条件为:以丙酮为溶剂,Na2CO3为缚酸剂,1 10 mmol,n(2)∶n(1)=2.4,于50℃反应6 h,产率98.1%。3的初始分解温度为292℃,700℃时成炭率34.5%。 相似文献
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β,β-二氯丁烯酮甲基上的反应 总被引:1,自引:0,他引:1
通过4,4-二氯-3-丁烯-2-酮的氯甲基化,Mannich反应和醇醛缩合制备了1,1,5-三氯-p-戊烯-3-酮(2),1,1-二氯-9-二乙胺基-1-戊烯-3-酮盐酸盐(3)和1,1-二氯-1,4-己二烯-3-酮(4).氯甲基化产品(2)与三乙胺在醚反应生成1,1-二氯-1,4-戊二烯-3-酮(6),在醇中生成1,1-二氯-5-乙氧基-1-戊烯-3-酮(6).与容易在室温中聚合.(2)和氨在醇中反应可得到环化产品N-(4-酮基-5H,6H-2-吡啶基)-3H,4H,5H-吡啶-2,4-二酮. 相似文献
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将1,3,4-噁二唑基团引入二芳基乙烯分子中, 合成了2种新的二芳基乙烯类光致变色化合物1-氰基-2-(2H-5-苯基-1,3,4-噁二唑)-1,2-二(2,4,5-三甲基-3-噻吩)乙烯(3)和1,4-二{[1-氰基-2-(2H-5-苯基-1,3,4-噁二唑)-1,2-二(2,4,5-三甲基-3-噻吩)乙烯]-1,3,4-噁二唑}苯(4). 通过IR, NMR, MS和元素分析对化合物进行了结构表征, 并研究了其UV-Vis吸收、荧光发射、动力学特性和抗疲劳性质. 实验结果表明, 化合物[STHZ]3[STBZ]和[STHZ]4[STBZ]具有良好的光致变色性质, 光致变色闭环反应为零级反应, 开环反应为一级反应. 相似文献
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制备了氯铂酸-异丙醇、氯铂酸-聚甲基乙烯基硅氧烷和氯铂酸-三苯基膦三种催化剂,评价了它们在乙炔与三乙氧基硅烷的硅氢加成反应中的催化活性及选择性;并考察了反应温度、乙炔流量、氯铂酸-聚甲基乙烯基硅氧烷与三乙氧基硅烷摩尔比、PPh3/H2PtCl6摩尔比等因素对产物收率的影响.结果表明,氯铂酸-聚甲基乙烯基硅氧烷对该反应表现出较高的催化活性,在催化剂与三乙氧基硅烷摩尔比为1.2×10-4∶1,T=80℃,乙炔流量=120 mL/min的条件下反应,产物乙烯基三乙氧基硅烷的选择性为100%,收率可达97.5%. 相似文献
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Hughes G Kreher D Wang C Batsanov AS Bryce MR 《Organic & biomolecular chemistry》2004,2(22):3363-3367
2-(4-tert-Butylphenyl)-5-(4-ethynylphenyl)-1,3,4-oxadiazole reacts with a series of heteroaryl iodides under standard Sonogashira cross-coupling conditions (Pd[PPh(3)](2)Cl(2), CuI, triethylamine, THF) to yield products 2a-g in 40-79% yields (heteroaryl = 2-pyridyl, 3-pyridyl, 4-pyridyl, 2-pyrazyl, 5-bromo-2-pyrimidyl, 2-thienyl and 3-thienyl, respectively). Compound 2f was lithiated followed by electrophilic iodination (BuLi, perfluorohexyl iodide) to give 3, which by a two-step sequence gave the terminal ethynylthienyl derivative 5. Conversion of 5 into the terminal ethynylaldehyde derivative 7, via acetal derivative 6, proceeded in high yield. Starting from 2-iodo-5-methoxycarbonylthiophene, a five-step sequence afforded 2-(4-tert-butylphenyl)-5-(4-ethynylthienyl)-1,3,4-oxadiazole 13 (13% overall yield). Reactions of 13 gave terminal pyridyl, pyrazyl, pyrimidyl and thienyl derivatives, analogous to those obtained from 1. Two-fold reaction of 13 with 2,5-diiodothiophene gave the bis(ethynylthienyl)thiophene derivative 15 (30% yield). Solution UV-Vis absorption and photoluminescence spectra establish that replacement of the phenyl ring in the 2,5-diphenyl-1,3,4-oxadiazole series 2a-g by a thienyl ring [i.e. the 2-phenyl-5-(2-thienyl)-1,3,4-oxadiazole series 14a-g] leads to a red shift in the lowest energy band in both the absorption spectra and emission spectra. The X-ray crystal structures of compounds 2d, 2g, 5 and 14d.CHCl(3) reveal that the molecular structures are approximately planar although there are substantial differences in the conformations. 相似文献
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Zhang Lixue 《高等学校化学研究》1989,(2)
By ring-closure of 1-nicotinyl-4-arylthiosemicarbazides under the catalysis of concentrated sulfuric acid or mercuric acetate, a series of 2-(3-pyridyl)-5-arylarnino-1,3,4-thiadiazoles and 2-(3-pyridyl)-5-ary-lamino-1,3,4-oxadiazoles were synthesized, respectively. All the products were subjected to testing of biological activity. Furthermore, the IR, 1H NMR and MS spectral properties of these new compounds were studied in details and some significant conclusions were drawn. 相似文献
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《Journal of Saudi Chemical Society》2014,18(2):101-106
In the present investigation, a series of 2(4-pyridyl)-5[(aryl/heteroarylamino)-1-oxoethyl]thio-1,3,4-oxadiazole were synthesized using isonicotinohydrazide and substituted aryl/heteroaryl amines using pyridine as solvent. Newly synthesized compounds were tested for their in vitro anti-tubercular activity against Mycobacterium tuberculosis H37Rv using the BACTEC 460 radiometric system. Among the synthesized compounds, compounds 2(4-pyridyl)-5((2-nitrophenylamino)-1-oxoethyl)thio-1,3,4-oxadiazole (5e), 2(4-pyridyl)-5((4-nitrophenylamino)-1-oxoethyl)thio-1,3,4-oxadiazole (5g) and 2(4-pyridyl)-5((2-pyrrolylamino)-1-oxoethyl)thio-1,3,4-oxadiazole (5k) produced highest efficacy and exhibited >90% inhibition at a concentration of 0.0077, 0.0052 and 0.0089 μM, respectively. All the new compounds were pharmacologically evaluated for their in vitro Antimicrobial activity. 相似文献
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合成了新的尾式-5-{2-[(5-溴-2-吡啶)偶氮-]5-(二乙氨基)苯氧基}对丁氧基苯基-10,15,20-三苯基卟啉{H2[5-Br-PADAPBPP]}及其Pd2 和Ni(bpy)2 配合物,其结构经UV,1HNMR,IR和元素分析表征。 相似文献
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Rafał Frański 《Journal of mass spectrometry : JMS》2004,39(3):272-276
The complexes of 2,5-disubstituted-1,3,4-oxadiazoles, namely 2,5-diphenyl-1,3,4-oxadiazole (1), 2,5-bis(2-pyridyl)-1,3,4-oxadiazole (2) and 2,5-bis(4-pyridyl)-1,3,4-oxadiazole (3), with copper cation were studied by electrospray ionization mass spectrometry (ESI-MS). The ability of the compounds studied to form complexes with copper (under the ESI conditions) can be ordered as 2 > 1 > 3. The compounds studied tend to form both 1 : 1 and 2 : 1 chelate complexes with both copper(II) and copper(I). The complexes with copper(I) are formed in the ESI process. The influence of solvent polarity, solution flow-rate, counter ions (Cl−, NO3−, CH3COO−, SO42−, acetylacetonates) on the type of the ions observed was studied. Copyright © 2004 John Wiley & Sons, Ltd. 相似文献
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2-Amino-and 2-hydrazino-5-(3 or 4-pyridyl)-1, 3, 4-oxadiazoles [IIi-k] have been prepared by racting 2-chloro derivatives with the corresponding amines or hydrazines, the 2-hydrazino (IIi-k) compounds that obtained were heated with carbon disulphide and alcoholic potassium hydroxide where 5-(3 or 4-pyridyl)-1,3,4-oxadiazolo (2,3-C)-1,2,4-triazole 5-thione (IIIa-c) were obtained, the given structures were biologically screened. 相似文献
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Ion chromatography has been applied to the determination of inositol 2,4,5-trisphosphate (Ins 2,4,5-P3), inositol 1,3,4-trisphosphate (Ins 1,3,4-P3), inositol 1,4,5-trisphosphate (Ins 1,4,5-P3), and inositol 1,3,4,5-tetrakisphosphate (Ins 1,3,4,5-P4). Other common polyanionic metabolites, including ATP and GTP, do not interfere with the determinations even at concentrations exceeding those normally found in tissue extracts. Assay of rat brain for Ins 1,4,5-P3 and Ins 1,3,4,5-P4 by the method of standard addition gives values which are within 10% of the amount calculated by external calibration. When rat brain homogenates are spiked with Ins 1,4,5-P3, the recoveries are greater than 90%. Treatment of animals with lithium chloride and pilocarpine produces increases in total inositol trisphosphates from 14 to 64 nMol/g wet weight, and increases in Ins 1,3,4,5-P4 from 0.9 to 18 nMol/g wet weight in tissue extracts obtained from the cerebral cortex. Using chemically suppressed conductivity, detection limits in brain are estimated to be 50 pMol/g wet weight for inositol trisphosphates and 22 pMol/g wet weight for inositol tetrakisphosphate. 相似文献
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The treatment of binuclear complexes [Cp*(2)M(2)(μ-QA)Cl(2)] (M = Ir, 2a; M = Rh, 2b) (H(2)QA = 1,4-dihydroxyanthraquinone) with pyrazine or bifuncational pyridyl-based ligands (4,4'-dipyridine (bpy), E-1,2-bis(4-pyridyl)ethene (bpe), 2,5-bis(4-pyridyl)-1,3,4-oxadiazole (bpo), and 2,5-bis(4-pyridyl)-1,3,4-thiadiazol (bpt)) in the presence of AgOTf (OTf = CF(3)SO(3)) in CH(3)OH, gave the corresponding tetra-nuclear complexes, with a general formula of [Cp*(4)M(4)(μ-QA)(2)(μ-L)(2)](OTf)(4) (M = Ir, 3a-7a; M = Rh, 3b-7b), respectively. The molecular structure of [Cp*(4)Ir(4)(μ-QA)(2)(μ-pyrazine)(2)](OTf)(4) (3a) has been determined by single-crystal X-ray analysis, revealing that the metal centers were connected by pyrazine and bis-bidentate QA(2-) ligands to construct a rectangular cavity with the dimension of 7.30 × 8.41 × 6.92 ?. Complexes 3a and 3b were found to exhibit selective trapping of halocarbons properties. 相似文献