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以1-甲基-3-乙基(-4-氯)-5-吡唑甲酰肼作原料,经两步得到4-氨基-3-(1-甲基-3-乙基(-4-氯)-5-吡唑基)-1,2,4-三唑-5-硫酮(3),3再与取代羧酸反应,得到一系列3-(1-甲基-3-乙基(-4-氯)-5-吡唑基)-6-取代均三唑并[3,4-b]-1,3,4-噻二唑(4、5、6).元素分析、1HNMR、IR和MS确定了它们的结构.初步生测结果表明:3具有植物生长调节活性,4b、4d、6具有杀菌活性. 相似文献
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Synthesis of 3,6-Disubstituted 5,6-Dihydro-s-triazolo [3,4-b]-1,3,4-thiadiazolidines through the Intramolecular Mannich Reaction 总被引:2,自引:0,他引:2
3-取代基-4-氨基-5-巯基-1,2,4-三唑在微量酸催化下与取代芳香醛经分子内Mannich反应合成了29个新的3,6-二取代-5,6-二氢-s-三唑并[3,4-b]-1,3,4-噻二唑啉类化合物,其结构经元素分析、IR和1HNMR进行确证,并讨论了反应的立体选择性。 相似文献
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用铜(Ⅱ)—L—精氨酸配体交换薄层色谱拆分氨基酸对映体 总被引:2,自引:0,他引:2
报道了一种新的配体交换薄层色谱拆分氨基酸对映体的方法。以醋酸铜-L-精氨酸的络合物为配体交换剂,用浸渍的方法吸附在硅胶薄层板上,制成配体交换薄层,用PRISMA优化法选择出展开剂的最佳组成为:甲醇/乙腈/四氢呋喃/水=80:8.2:5.8:6,在此色谱条件下,十对氨基酸对映体得到良好的分离,D-和L-氨基酸的相对比移值在1.09-2.40之间。文中对配体交换薄层的制备方法,样品的分子结构及色谱行为 相似文献
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在pH4.0的介质中,Mo(Ⅵ)与新试剂4-(5-溴-2-噻唑偶氮)邻苯二酚(5-Br-TAPC)和二苯胍(DPG)反应形成稳定的三元离子缔合物,其组成比Mo(Ⅵ):5-Br-TAPC∶DPG为1∶3∶2。该三元缔合物氯仿萃取液的λmax为536nm,对比度为119nm,表观ε为6.33×104L·mol-1·cm-1。钼(Ⅵ)含量在0~0.80mg/L范围内遵从比耳定律,并探讨了离子缔合物的结构。将在最佳显色条件下拟定的分析方法用于合金钢中小量或痕量钼的测定,取得了满意的结果。 相似文献
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1 引 言 DBC-偶氮氯膦全称为:2-(4-氯-2-膦酸基苯偶氮)-7-(2,6-二溴-4-氯苯偶氮)-1,8-二羟基3,6-萘H磺酸,简写为DBC-CPA。它已用于稀土、钡、锶、钙和钐的测定。作者在研究了该试剂与铁显色反应的基础上,又研究了与铋的显色反应,发现在1.2moL/L HClO4的介质中,于少量乙醇存在下,试剂与铋生成2:1的络合物,络合物稳定性好,灵敏度高,其表观摩尔吸光系数 1.08× 105 L·mol-1·cm-1,常见离子:银、镁、镉、钴、镍、铜、锰、铝、锌、铁、铬、硅等允许共… 相似文献
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5-芳基-2-呋喃甲酸及其衍生物具有调节植物生长等作用[4].我们通过大量的实验,选用PTC法,利用5-芳基-2-呋喃甲酰氯与芳胺和芳氧基乙酰肼反应,合成了新化合物Ⅱ和Ⅳ:RCOClO(Ⅰ)ArNH2/PEG-400→RCONHAr(Ⅱ)ONaOH/... 相似文献
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二唑衍生物具有抗菌、消炎和调节植物生长等活性[1~5].二唑硫醚衍生物也具有一定抗菌活性[6].为筛选具有生物活性的新化合物和研究亲核取代反应的规律,我们设计和合成了新的2-酰肼基-5-(2,4-二氯苯基)-1,3,4-二唑2,研究了2在K2C... 相似文献
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Reactions between the three components Ag2O, V2O5, and HF(aq) were investigated under hydrothermal conditions, and the recovered phases were, in increasing Ag:V content, Ag2V4O11, beta-AgVO3, Ag4V2O6F2, Ag4V2O7, and alpha-Ag3VO4. A higher ratio of Ag2O to V2O5, as compared to a stoichiometric ratio, was required to synthesize Ag4V2O6F2, Ag4V2O7, and alpha-Ag3VO4. Owing to their solubility differences, the crystallization regions are not centered around the respective 2:1 and 3:1 Ag2O/V2O5 tie-lines but rather are centered along the 4:1 and 8:1 Ag2O/V2O5 tie-lines. Reactions with a 4:1 Ag/V ratio either resulted in Ag4V2O6F2 at 150 degrees C or Ag4V2O7 at 200 degrees C. Products were recovered in between 80% and 100% yield based on V2O5. Red transparent crystals of alpha-Ag3VO4 crystallize in the monoclinic space group C2/c, with cell parameters a = 10.1885(16) A, b = 4.9751(8) A, c = 10.2014(17) A, beta = 115.754(3) degrees . 相似文献
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A novel {V(4)Nb(6)O(30)} addenda: Through the successful introduction of a vanadium atom into the polyoxoniobate system, three novel compounds containing the same unprecedented mixed addenda vanadoniobate cluster {V(4)Nb(6)O(30)} were obtained. The incorporation of suitable atoms like V is an intriguing subject providing vast possibilities to enrich polyoxoniobate chemistry. 相似文献
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Yucesan G Golub V O'Connor CJ Zubieta J 《Dalton transactions (Cambridge, England : 2003)》2005,(13):2241-2251
The hydrothermal reactions of CuSO4.5H2O, Na3VO4, 2,2':6':2'-terpyridine (terpy), and the appropriate organophosphonate ligand yield a series of materials of the Cu(ii)-terpy/oxovanadium organophosphonate family. The complexes exhibit distinct structures spanning one-, two- and three-dimensions and exhibiting diverse oxovanadium building blocks. Thus, [{Cu(terpy)}(V2O4)(O3PPh)(HO3PPh)2] (1) is one-dimensional and constructed from binuclear units of corner-sharing V(v) square pyramids. While [{Cu(terpy)}VO(O3PCH2PO3)] (2), [{Cu(terpy)}2(V4O10)(O3PCH2CH2PO3)] (3), and [{Cu(terpy)}(V2O4){O3P(CH2)3PO3}].2.5H(2)O (4.2.5H2O) are similarly one-dimensional, the V/O structural components consist of isolated V(iv) square pyramids, tetranuclear V(v) units of three tetrahedra and one square pyramid in a corner-sharing arrangement, and isolated V(v) tetrahedra and square pyramids, respectively. The second propylenediphosphonate derivative, [{Cu(terpy)}(V2O4){O3P(CH2)3PO3}] (5) is three-dimensional and exhibits isolated V(v) tetrahedra as the vanadate component. The two-dimensional structure of [{Cu(terpy)(H2O)}(V3O6){O3P(CH2)4PO3}] (6) is mixed valence with isolated V(iv) square pyramids and binuclear units of corner-sharing V(v) tetrahedra providing the V/O substructures. 相似文献
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Several novel mono( ?-enaminoketonato) vanadium complexes bearing constrained cyclic skeleton, including[(C6H5)C6H3C(O) = C(CH2)nCH = N ― Ar]VCl2(THF)2(V3a: n = 1, Ar = C6H5; V4a: n = 2, Ar = C6H5; V4b: n = 2, Ar =C6F5; V4c: n = 2, Ar =(C3H7)2C6H3; V5a: n = 3, Ar = C6H5), were synthesized and their structure and properties were characterized. The structures of V4 c and V5 a in solid-state were further confirmed by X-ray crystallographic analysis.Density functional theory(DFT) results indicated that these complexes showed enhanced steric hindrance around the metal center as compared with the acyclic analogues. Upon activation with Et2 Al Cl and in the presence of ethyl trichloroacetate as a reactivator, all of the complexes exhibited high catalytic activities(107 g PE/(mol V·h)) toward ethylene polymerization, and the obtained polymers exhibited unimodal distributions(Mw/Mn = 2.0-2.3) even produced at elevated temperatures(70-100 °C) and prolonged reaction time. When MAO was employed as a cocatalyst, they only showed moderate catalytic activities(105 g PE/(mol V·h)), but the resulting polymers had higher molecular weights(168-241 kg/mol). These vanadium complexes with cyclic skeleton also showed high catalytic activities toward ethylene/norbornene copolymerization. The produced copolymers displayed approximate alternating structure at high in-feed concentration of norbornene. The catalytic capabilities of these complexes could be tuned conveniently by varying ligand structure. Furthermore, the cyclic voltammetry results also proved that these complexes exhibited better redox stabilities than the complexes bearing linear skeleton. 相似文献
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Hydrothermal reactions of the V2O5/2,2':6':2"-terpyridine/ZnO/H2O system under a variety of conditions yielded the organic-inorganic hybrid materials [V2O4(terpy)2]3[V10O28].2H2O (VOXI-10), [VO2(terpy)][V4O10] (VOXI-11), and [V9O22(terpy)3] (VOXI-12). The structure of VOXI-10 consists of discrete binuclear cations [V2O4(terpy)2]2+ and one-dimensional chains [V10O28]6-, constructed of cyclic [V4O12]4- clusters linked through (VO4) tetrahedra. In contrast, the structure of VOXI-11 exhibits discrete mononuclear cations [VO2(terpy)]1+ and a two-dimensional vanadium oxide network, [V4O10]1-. The structure of the oxide layer is constructed from ribbons of edge-sharing square pyramids; adjacent ribbons are connected through corner-sharing interactions into the two-dimensional architecture. VOXI-12 is also a network structure; however, in this case the terpy ligand is incorporated into the two-dimensional oxide network whose unique structure is constructed from cyclic [V6O18]6- clusters and linear (V3O5(terpy)3) moieties of corner-sharing vanadium octahedra. The rings form chains through corner-sharing linkages; adjacent chains are connected through the trinuclear units. Crystal data: VOXI-10, C90H70N18O42V16, triclinic P1, a = 12.2071(7) A, b = 13.8855(8) A, 16.9832(10) A, alpha = 69.584(1) degrees, beta = 71.204(1) degrees, gamma = 84.640(1) degrees, Z = 1; VOXI-11, C15H11N3O12V5, monoclinic, P2(1)/n, a = 7.7771(1) A, b = 10.3595(2) A, c = 25.715(4) A, beta = 92.286(1) degrees, Z = 4; VOXI-12, C45H33N9O22V9, monoclinic C2/c, a = 23.774(2) A, b = 9.4309(6) A, c = 25.380(2) A, beta = 112.047(1) degrees, Z = 4. 相似文献
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A novel compound Ni(phen)(H2O)(V2O6) has been hydrothermally synthesized and structurally determined to be a two-dimensional compound, which contains {V2O6}n2n- chains interconnected by nickel(Ⅱ) complexes via oxygen atoms. The crystallographic data measured by single-crystal X-ray diffraction analysis are as follows: C12H10N2NiO7V2, Mr=454.81, monoclinic, space group P21/c, a=0.784 6(3), b=2.103 6(8), c=0.942 3(4) nm, β=112.872(5)°, V=1.433 0(10) nm3, Z=4, Dc=2.104 Mg·m-3, μ(Mo Kα)=2.615 mm-1, F(000)=904, T=298(2) K, 4 480 reflections collected, 2 470 independent (Rint=0.032 2), the final R=0.058 4 and wR2=0.145 7 for 2 303 observed reflections with I>2σ(I). CCDC: 192520. 相似文献
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