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1.
以磷酰胺氮芥为药效基团,对甲苯磺酰胺为载体,通过乙二胺的连接方式,合成了14个新型含磺酰基的磷酰胺氮芥衍生物,其结构经1H NMR,13C NMR,31P NMR和元素分析表征. 相似文献
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首次合成了氟芳胺基磷酸酯和氟磺酰胺基磷酸酯.对氟苯胺、α-氯-4-三氟甲基吡啶胺、α-氯-4-三氟甲基氧化吡啶胺与二乙氧基磷酰氯在乙腈或DMF中反应,得到氟芳胺基磷酸酯.氟烷基磺酰甲胺与二乙氧基磷酰氯反应,以金属钠处理,相应钠盐在乙腈或DMF中,于室温下反应将得到氟烷磺酰胺基磷酸酯. 相似文献
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N,N′,N″—三(对—甲苯磺酰基)二亚乙基三胺与氢化钠反应生成二钠盐,然后与N,O,O'—三(对—甲苯磺酰基)双(2—羟乙基)胺进行缩合环化反应,得N—对甲苯磺酰化的四氮杂环十二烷。在浓H_2SO_4作用下,脱去对—甲苯磺酰基,最后得到了1,4,7,10—四氮杂环十二烷,总得率为44%。 相似文献
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以N-对甲苯磺酰基乙二胺、取代醛、芳酮及亚磷酸酯为原料,采用“一锅煮”合成了一系列新型的含磺酰基的α-氨基磷酸酯,其结构经1H NMR,13C NMR,31P NMR和元素分析表征. 相似文献
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磺酰氨基酸钛配合物对Diels-Alder反应的对映选择性催化作用 总被引:3,自引:0,他引:3
研究了对甲苯磺酰基-L-缬氨酸、对甲苯磺酰基-L-苯丙氨酸、对甲苯磺酰基-L-亮氨酸、对甲苯磺酰基-L-异亮氨酸、对甲苯磺酰基-L-脯氨酸、1-萘磺酰基-L-缬氨酸、1-萘磺酰基-L-苯丙氨酸、1-萘磺酰基-L-亮氨酸和1-萘磺酰基-L-异亮氨酸与钛的配合物对环戊二烯与丙烯酸甲酯的环加成反应的对映选择性催化作用。萘磺酰基氨基酸钛配合物的对映选择性比对甲苯磺酰基氨基酸钛配合物好,氨基酸与钛比为2:1时比1:1要好得多。1-萘磺酰基-L-异亮氨酸与钛的2:1配合物的对映选择性最好,e.e.值为56%。 相似文献
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介绍了带羟基桥连双-(中环多胺)的合成,首先利用N-对甲苯磺酰基-3-羟基-1,5-二杂环庚烷与5种双官能基化合物在N2气氛下无水乙腈中反应,得到5种带对甲苯磺酰基的中环多胺,然后利用HBr/HOAc脱去保护基团,得到桥连双-(中环多胺)的氢溴酸盐,所有新化合物的结构均经IR,^1HNMR,MS或元素分析证实。 相似文献
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A novel efficient synthetic method for 2,2',3,3'-biphenyltetracarboxylic dianhydride 总被引:1,自引:0,他引:1
A novel approach to the synthesis of 2,2',3,3'-biphenyltetracarboxylic dianhydride is described. The target compound was prepared by a nickel-catalyzed coupling reaction of dimethy 3-chlorophthalate (3-DMCP) for 4 h at 70-80℃, followed by subsequent hydrolysis of tetra-ester in acid solution and dehydration of tetra-acid, with overall yield of 68%. The structures of the products were characterized by IR, 1H NMR and 13C NMR respectively. 相似文献
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The allomerization of chlorophyll b in methanol produced 132(S)-hydroxy-10-methoxychlorophyll b in a yield of ca. 8%. The formation of this allomer was totally unexpected, as 10-substituted chlorophylls have never been reported before. The structure of the new chlorophyll b derivative was determined on the basis of UV/Vis, FAB-MS, 1H NMR and 2D ROESY NMR spectra. This letter focuses on the NMR analysis. 相似文献
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João Paulo R.F. André Hugh D. Burrows Carlos F.G.C. Geraldes Maria Da Graça M. Miguel M.Helena S.F. Teixeira L.F. Vilas Boas 《Polyhedron》1996,15(24):4331-4340
Complexation of europium(III) with glyceryl-1- and -2-phosphates has been studied by metal ion luminescence, 1H and 13C NMR spectroscopy and potentiometry. From the luminescence and NMR studies, the formation of a 1:1 inner-sphere complex, in which the glyceryl phosphate is directly bound to the metal, is confirmed. Similar apparent binding constants at pH 2 were obtained by the three methods. Values obtained by NMR at pH 2 are 53 M−1 and 12 M−1 for glyceryl-1- and -2-phosphate, respectively. By comparison with literature data on related systems it is suggested that the ligands bind through the phosphate group. To obtain structural information from the NMR data, complexation has also been studied with the lanthanide ions Dy(III), Er(III) and Gd(III) using both chemical shift and relaxation data. From this, metal-proton distance ratios have been calculated. Comparison of 1H and 13C NMR spectral data in the presence of paramagnetic lanthanides suggests conformational equilibria in the solutions. From the potentiometric studies, global formation constants have been determined, and speciation diagrams obtained over the pH range 1.5pH7.0 for ligand/metal ratios of 1 and 30. Implications of these results on lanthanide induced fusion of phospholipid membranes are discussed. 相似文献
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Koichi Komatsu Yasujiro Murata Nobuyuki Sugita Ken'ichi Takeuchi Terence S. M. Wan 《Tetrahedron letters》1993,34(52):8473-8476
A reaction of C60 with an equimolar amount of anthracene in refluxing naphtlhalene gives the 1:1 Diels-Alder adduct in 67% yield based on consumed C60: the adduct was fully characterized by IR, UV-vis, 1H and 13C NMR, and MS spectroscopy, and exhibited reversible reduction waves at the potential 0.11 to 0.19 V more negative and an irreversible oxidation peak at the potential 0.11 V less positive than those of C60 itself. 相似文献
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E. K. Foord J. Cole M. J. Crawford J. W. Emsley G. Celebre M. Longeri J. C. Lindon 《Liquid crystals》1995,18(4):615-621
The 1H, 2H and 13C NMR spectra of phenyl acetate, phenyl acetate-[13CO] and phenyl acetate-[C2H3] dissolved in a nematic liquid crystalline solvent have been analysed to yield dipolar coupling, Dij. These have been interpreted using the additive potential model to provide information on the molecular conformation, resulting in three possible shapes for V(φ), the potential energy for rotation about the ring-oxygen bond. A comparison with the results of molecular orbital calculations leads to the conclusion that a potential with a minimum at 54.4° ± 0.1° is the most probable. 相似文献
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手性膦酸二酯类化合物的合成与结构 总被引:3,自引:0,他引:3
手性呋喃酮1a1b与亚磷酸三酯2a2b通过串联的不对称Michael加成/分子内Michalis-Arbazov重排反应,得到含磷官能团的新手性化合物5-(S)-(1S)-冰片氧基-4-膦酸二酯基-3-卤素-2(5H)-呋喃酮(3a~3d).该反应具有条件温和,产率高(69%~93%),光学纯度单一(d.e.≥98%)等特点.通过元素分析,IR,UV1HNMR13CNMR,MS,[α]D20等分析数据以及X射线四圆衍射确定了它们的化学结构和绝对构型. 相似文献
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以D-甘露醇为原料,经缩合,醇解,叠氮化和还原等4步反应制得含联1,3-二氧六环骨架的手性胺中间体(4); 4分别与3,5-双(三氟甲基)苯基异硫氰酯,表奎宁异硫氰酸酯和表奎尼丁异硫氰酸酯偶联合成了3个新型的手性硫脲(6a~6c),其结构经1H NMR, 13C NMR, IR和HR-MS表征。以硝基甲烷和苯甲醛的不对称Henry反应为探针反应,考察了6的催化活性。结果表明:在以吡啶为碱,甲苯为溶剂,6b 5%(摩尔百分数),于-30 ℃反应24 h的条件下,(S)-2-硝基-1-苯基乙醇的收率和对映选择性分别为69%和78%。 相似文献
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Zhu Yinghuai Shirley Lo Pei Sia Fethi Kooli Keith Carpenter Richard A. Kemp 《Journal of organometallic chemistry》2005,690(26):6284-6291
In situ reaction of Li[closo-1-Ph-1,2-C2B10H10] with 7-azabicyclo [4.1.0] heptane results in the formation of the disubstituted carborane, closo-1-Ph-2-(2′-aminocyclohexyl)-1,2-C2B10H10 (1), in 63% yield. Decapitation of (1) with potassium hydroxide in refluxing ethanol produces the cage-opened nido-carborane, K[nido-7-Ph-8-(2′-aminocyclohexyl)-7,8-C2B9H10]− (2), in 80% yield. Deprotonation of the above monoanion with two equivalents of n-butyllithium followed by reaction with anhydrous MCl4 · 2THF (M = Zr, Ti) provides d0-half-sandwich metallocarboranes, closo-1-M(Cl)-2-Ph-3-(2′-σ-(H)N-cyclohexyl)-2,3-η5-C2B9H9 (3 M = Zr; 4 M = Ti) in 53% and 42% yields, respectively. The reaction of Li[closo-1,2-C2B10H11] with 7-azabicyclo [4.1.0] heptane in THF affords closo-1-(2′-aminocyclohexyl)-1,2-C2B10H10 (5) in 59% yield. Immobilization of the carboranyl amino ligand (1) to an organic support, Merrifield’s peptide resin (1%), has been achieved by the reaction of the sodium salt of (5) with polystyryl chloride in THF to produce closo-1-(2′-aminocyclohexyl)-2-polystyryl-1,2-C2B10H10 (6) in 87% yield. Further reaction of the dianion derived from (6) with anhydrous ZrCl4 · 2THF led to the formation of the organic polystyryl supported d0-half-sandwich metallocarborane, closo-1-Zr(Cl)-2-(2′-σ-(H)N-cyclohexyl)-3-polystyryl-2,3-η5-C2B9H9 (7), in 38% yield. These new compounds have been characterized by elemental analyses, NMR, and IR spectra. Polymerizations of both ethylene and vinyl chloride with (3) and (7) have been performed in toluene using MMAO-7 (13% ISOPAR-E) as the co-catalyst. Molecular weights up to 32.8 × 103 (Mw/Mn = 1.8) and 9.5 × 103 (Mw/Mn = 2.1) were obtained for PE and PVC, respectively. 相似文献
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应用串联氮杂Wittig反应设计合成了一系列新的2-烷氨(芳氧)基-3,8-二苯基-5-芳基-6-甲基-5,8-二氢-4H-吡唑并[4',3':5,6]吡喃并[2,3-d]嘧啶-4(3H)-酮衍生物。通过氢核磁共振谱仪(1H NMR)、傅里叶变换红外光谱仪(FTIR)和元素分析等方法对所合成的化合物进行了结构表征,用X射线单晶衍射确证了化合物2-二正丙基氨基-3,8-二苯基-5-(4-甲基苯基)-6-甲基-5,8-二氢-4H-吡唑并[4',3':5,6]吡喃并[2,3-d]嘧啶-4(3H)-酮(Ⅲi)晶体结构。室内的杀菌和杀虫活性测试结果表明:目标化合物具有一定的杀菌活性,其中部分化合物对黄瓜灰霉菌(Botrytis cinereapers)在50 mg/L剂量下抑制率达到90%以上,显示了优异的杀菌活性;对水稻褐飞虱无明显的杀虫活性,但发现对粘虫具有较高的杀灭效果,大多数抑制率达到90%以上。 相似文献