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1.
采用毛细管气相色谱法对间接电氧化法合成的二甲砜及反应物二甲亚砜进行了分离分析。研究了分离二甲砜、二甲亚砜的最佳条件,内标法定量。两种化合物的线性范围在2-30μg,且有较好的精密度。 相似文献
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A. W. BERGER † J. N. DRISCOLL † J. S. DRISCOLL J. A. PIROG § H. LINSCHITZ| 《Photochemistry and photobiology》1968,7(5):415-420
The chemiluminescent autoxidation of over fifty indoles has been measured in dimethyl sulfoxide (DMSO). The 3-alkylindole derivatives represent the brightest and most efficient members of this group. The chemiluminescence yield (per mole) of skatole is (1·5 ± 0·6) × 10-3. The chemiluminescence spectrum of skatole is identical with the fluorescence spectrum of o-formamidoacetophenone in the same environment Similar results for 2,3-dimethylindole lead to the identification of the acylamide anion as the emitter in indole chemiluminescence. A peroxide ring cleavage excitation mechanism is proposed. 相似文献
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[Nd(DMSO)_5(H_2O)_3]Cl_3·H_2O的单晶用ENRAF-NONIUS CAD 4型四圆衍射仪收集衍射数据进行结构分析,最终偏离因子R=0.036。晶体属三斜晶系空间群P_1,晶胞参数a=9.800(1),b=10.531(1),c=14.757(2);α=93.07(1),β=100.2l(1),γ=99.71(1)°;Z=2。结构分析证实:晶胞中有二个[Nd(DMSO)_5(H_2O)_3]Cl_3·H_2O分子。Nd与五个DMSO及三个H_2O中的氧形成八配位的畸变三角十二面体结构。Cl~-与络阳离子通过离子键相互作用。[Tb(DMSO)_5(H_2O)_3)Cl_3·H_2O的晶胞参数与之相近,有类似的结构。 相似文献
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Abstract The chemical and biological importance of DMSO and other sulfoxides is partly due to the wide variety of molecular complexes formed with these molecules(1). The relatively large dipole moment of DMSO and the peculiar conformational properties of the sulfoxide moiety facilitates the formation of such complexes. There is experimental evidence that the formation of the molecular complex may be accompanied by extensive geometrical distortions of the DMSO molecule (2). 相似文献
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《Journal of Coordination Chemistry》2012,65(3):135-141
Abstract Amino acid complexes of general formula K[Pt(NO)Cl2], where NO denotes the metal bonded atoms of the amino acid, react completely with solvent DMSO to yield two products, cis- and trans-Pt(NO) (DMSO)Cl, where cis and trans refer to positions of DMSO relative to coordinated nitrogen. The products were identified and kinetic data were obtained from changes in the proton nmr spectra of the amino acid, when DMSO-d6 was the solvent, or of both amino acid and coordinated DMSO, when ordinary DMSO was the solvent. For glycine and π-aminoisobutyric acid complexes, the rate of displacement of trans chloride exceeds that of cis chloride by a factor of 3. However, subsequent equilibration favors the cis isomer over the trans isomer by a factor of 10. By contrast, for the corresponding N, N-dimethyl derivatives, the rates of formation of the two isomers are more nearly the same and the equilibrium ratio does not differ from the kinetic ratio. In addition to providing a sensitive technique for evaluating small differences in kinetic trans-effects, these observations strongly suggest that the stereochemistry of Pt(NO) (DMSO)Cl for the corresponding alanine complex described by Kukushkin and Guryamava should be denoted cis, rather than the trans reported. 相似文献
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<正> A new series of hexatungstate compounds has been prepared recently in this laboratory. The starting material is white powdery tungstic acid,and its extraction solution by DMSO reacts with many transition metal carbonates to give the hexatungstates of the respective metallic ions coordinated by DMSO. Among them,the structures of hex-akis(dimethylsulfoxide)-manganese (Ⅱ) hexatungstate [{(CH3)2SO}6Mn] [W6O19](1) and hexakis(dimethyl sulfoxide)-copper(Ⅱ) hexatungstate [{(CH3)2SO}6Cu}][W6O19] (2) have been determined from three-dimensional x-ray diffraction data and are hereby reported.Both compounds (1) and (2) crystallize in the monoclinic space group C2/c. The u-nit cell parameters for compound (1) are α=16. 398(3),b= 15. 026(1) ,c= 17. 827(2) A,β=111. 84(2)°,Z=4;and those for compound (2) are α=19. 165(4) ,b=14. 131 (2),c=16. 626(4) A ,β=117. 40(2)°, Z= 4. Both structures were solved by direct methods. Full matrix least squares refinements of positional and anisotropic temperature factors based o 相似文献
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Alan Queen A. F. Janzen A. Lemire K. Preston. 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-2):251-252
Abstract The reaction of an alkyl chloroformate with dimethyl sulfoxide gives the corresponding alkoxysulfonium chloride (I; X = 0) and carbon dioxide. However, the corresponding reactions with chlorothiolformate esters do not yield the salts (I; X = S). Phenyl chlorothiolformate reacts with dimethyl sulfoxide according to equation [1]. 相似文献
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Shigeru Oae Takashi Takeda Tsutomu Kawai Naomichi Furukawa 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3-4):133-137
Abstract In the reaction of benzyl 2-pyridyl sulfoxide (1) with C6H5CH2MgCl, the incoming Grignard reagent tends to couple preferentially with 2-pyridyl group at lower temperatures, whereas, at higher temperatures, coupling between benzyl and 2-pyridyl groups with 1 tends to increase due presumably to the relatively more facile pseudorotation2 at higher temperatures. 相似文献
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D. K. Padma S. K. Vijayalakshmi A. R. Vasudeva Murthy 《Phosphorus, sulfur, and silicon and the related elements》2013,188(2):129-130
Abstract Solid complexes of thiophosphoryl fluoride and thiophosphoryl chloride with dimethyl sulphoxide (DMSO) have been prepared and characterized. 相似文献
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本文用紫外分光光度法首次跟踪研究了壳脑酸二甲酯(dimethl Shellolate)与溴加成反应的规律。结果表明该反应符合二级反应规律。其中自由基反应接近2/3。极性历程占1/3强:该反应活化能为66.8kJ/mol,为室温下便可发生的反应:盐效应可以在一定程度上阻滞反应。 相似文献
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K. Troev E. Tashev G. Borisov 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3):313-318
Abstract The transesterification process of dimethyl and diethyl phosphite with 1,3-dichloropropanol-2 is examined. It is found that the reaction proceeds in the absence of catalyst at a temperature of 155°, whereas in the presence of morpholine as a catalyst it takes place at 126°C. The transesterification of dimethyl phosphite and diethyl phosphite with 1,3-dichloropropanol-2 is accompanied by the evolution of dimethyl and diethyl ethers and alkyl halides (methyl chloride and ethyl chloride). 相似文献
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Characteristic chlorophyll (Chl) a aggregates formed in aqueous dimethyl sulfoxide (DMSO) were investigated spectroscopically. Four chlorophyll forms were found with increasing DMSO concentration; they are called A-672, A-683, A-695 and A-665 according to the wavelengths of their absorption maxima. Transformation occurred only in this order. Reverse transformation could not be realized. A-683 and A-695 were apparently formed by the interaction of Chl a with DMSO in the linear dimer and linear polymer arrangements, respectively. Coordination of the Mg atom with a DMSO O atom and interaction between the S atom of one DMSO molecule and the O atom of an other DMSO molecule should lead to formation of a sandwich-type complex of partially overlapping chlorophyll macrocycles (Chl a-DMSO)n. A-672 and A-665 were assigned to Chl a micelles and to dissolved monomeric Chl a in DMSO, respectively. Fluorescence spectra showed that the A-683 was highly fluorescent, while the A-695 was less fluorescent. Energy migration within the A-695 form to a trap with a low fluorescence yield might be responsible for this difference in the emission intensity. 相似文献
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《结构化学》1987,(3)
<正> InC12H8N2(CH3)2SOCl3, Mr=477.5, Triclinic, P1, a=7.640(1), b=9.907(2), c=12.250(2)A,α=94.26(2),β=96.61(1),γ=105.19(2), V=883.6A3,Z=2, Dc=1.795g·cm-3.μ(MoKα)=18.9cm-1, 293K. The structure was solved by heavy-atom method and refined to R=0.028 for 3026 observed reflections with I>3α(I). 相似文献
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用高分辨电子能量损失谱(HREELS~*)对CH_3CN(乙腈)及C_6H_5CN(苯基氰)在清洁与氧覆盖的Cu(111)及Pd(100)表面上的吸附及其反应进行了研究。从198 K时CH_3CN吸附在Cu(111)及Pd(100)表面上的高分辨电子能量损失谱(HREELS)中观察到v(C≡N)几乎消失, 并在195 meV处出现一个较弱的v(C=N)谱带, 表明CH_3CN在吸附过程中C≡N再杂化为C=N,C,N原子分别与金属表面原子键合并C=N平行于表面。从198 K时C_6H_5CN在Pd(100)及Cu(111)上的HREELS表明C_6H_5CN的环平面与CN平行于金属表面。在185K时C_6H_5CN在氧覆盖的Pd(100)表面上的HREELS与其在清洁表面上的相似。并未观察到覆盖氧增强了C_6H_5CN在Pd(100)上的吸附及其它效应。C_6H_5CN吸附在氧覆盖的Cu(111)表面上产生了C_6H_5CNO的特征谱带。 相似文献
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磷酸脲可作为反刍动物饲料添加剂和青贮饲料保藏剂,高浓度NP复合肥、聚磷酸和净化湿法磷酸的中间体,以及阻燃剂、清洗剂等。国外众多研究者对磷酸脲结构、性能和应用进行了广泛的研究。但对磷酸脲离解反应的热力学研究甚少,尚未见详尽报道。本文就磷酸脲 相似文献
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以内型3,3-二甲基-2-降冰片基乙醛(1)与叔丁胺反应制得醛亚胺(2),依次和溴化乙基镁,碘乙烷反应制得内型2-(3,3-二甲基-2-降冰片基)丁醛的亚胺(4),再经水解得内型2-(3,3-二甲基-2-降冰片基)丁醛(5)。后者经与乙二醇缩醛化及氧化分别制得该醛的缩醛(6)及羧酸(7)。这些化合物均为新化合物,经纯化后进行了结构分析,并对其质谱进行了讨论。 相似文献