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71.
The systems AeAl(2-x)Mgx (Ae = Ca, Sr, Ba) display electron concentration induced Laves phase structural changes. However, the complete sequence MgCu2 --> MgNi2 --> MgZn2 with increasing x (decreasing electron count) is only observed for Ae = Ca. Compounds SrAl(2-x)Mgx (0 < x < or = 2) and BaAl(2-x)Mgx (x = 0.85 and 2.0) were synthesized and structurally characterized by X-ray diffraction experiments. For the Sr system the structural sequence CeCu2 --> MgNi2 --> MgZn2 occurs with increasing Mg content x. Thus, larger Sr does not allow the realization of the MgCu2 structure at low x. For Ae = Ba a binary compound BaAl2 does not exist, but more Ba-rich Ba7Al13 forms. The reinvestigation of the crystal structure of Ba7Al13 by selected area and convergent beam electron diffraction in a transmission electron microscope revealed a superstructure, which subsequently could be refined from single X-ray diffraction data. The formula unit of the superstructure is Ba21Al40 (space group P31m, Z = 1, a = 10.568(1) angstroms, c = 17.205(6) angstroms). In Ba21Al40 a size match problem between Ba and Al present in Ba7Al13 is resolved. The structure of Ba7Al13 (Ba21Al40) can be considered as a Ba excess variant of the hexagonal MgNi2 Laves phase type structure. An incommensurately modulated variant of the MgNi2 structure is obtained for phases BaAl(2-x)Mgx with x = 0.8-1. At even higher Mg concentrations a structural change to the proper MgZn2 type structure takes place. 相似文献
72.
Christel Hempen Liane Glsle-Schwarz Ulrich Kunz Uwe Karst 《Analytica chimica acta》2006,560(1-2):35-40
Telmisartan is an angiotensin II receptor antagonist and a known drug against high blood pressure. In this report, the development of a new and rapid analytical technique, an enzyme-linked immunosorbent assay (ELISA) for the determination of telmisartan in human blood plasma is described. The immunoassay is based on a conversion of 4-(N-methylhydrazino)-7-nitro-2,1,3-benzooxadiazole (MNBDH) to 4-(N-methylamino)-7-nitro-2,1,3-benzooxadiazole (MNBDA), which is detected by fluorescence spectroscopy. The limit of detection was 0.1 ng/mL, the limit of quantification was 0.3 ng/mL and the working range extended from 0.3 ng/mL to 300 ng/mL. 相似文献
73.
Ulrich Schllkopf 《Angewandte Chemie (International ed. in English)》1977,16(6):339-348
Being both nucleophilic and electrophilic, α-metalated isocyanides can add to polar double bonds, forming heterocycles. They are also synthons for α-metalated primary amines. This article describes recent or improved procedures for their use in organic synthesis: (1) In heterocyclic syntheses to give 2-oxazolines, 2-imidazolines, 2-thiazolines, oxazoles and oligooxazoles, thiazoles, triazoles, imidazolinones, pyrroles, 5,6-dihydro-1,3-oxazines and -thiazines, and (via cycloaddition with nitrones) 2-imidazolidinones. (2) In the field of formylaminomethylenation, for example transformation of estrone methyl ether and a keto sugar into the corresponding α-formylaminoacrylic esters, and the conversion of aldehydes and ketones by 3- and 4-pyridyl-methyl isocyanides into N-(1-pyridyl-1-alkenyl)formamides and their hydrolysis to 3- and 4-acylpyridines. (3) In connection with the use of α-metalated isocyanides as synthons for α-metalated primary amines, the author demonstrates how they may be used for preparation of 1,2- and 1,3-amino alcohols, 1,2-diamines, 2,3-diaminoalkanoic acids and for synthesis of higher amino acids starting from simple amino acids. 相似文献
74.
Original mass spectra of uracil and thymine derivatives are presented with the corresponding fragmentation schemes. In the first series of spectra, the fragmentations of thymine derivatives, including 14C-2-thymine, dimers, and bromo thymines, confirm the basic retro Diels-Alder mechanism. The second series includes dihydro 5,6-derivatives of uracil (hydroxy and bromo substituents). The behaviour of these molecules is quite different; they are more sensitive to the substituents and a part of the fragmentation is often explained by protonated molecular ions. 相似文献
75.
Joachim Pump Eugene G. Rochow Ulrich Wannagat 《Monatshefte für Chemie / Chemical Monthly》1963,94(3):588-598
Zusammenfassung Durch Umsetzung von Disilbercyanamid mit Organyl- und Alkoxy-halogensilanen wurden 9 bisher unbekannte zweifach silylsubstituierte Carbodiimide der Stoffgruppen (R3SiN)2C, [(RO)3SiN]2C, (R2RSiN)2C und R3SiNCNSiR3 dargestellt und in ihrer Struktur über14N- und1H-kernmagnetische Resonanzmessungen, IR- und Raman-Spektren eindeutig als Carbodiimidderivate aufgeklärt.20. Mitt.:U. Wannagat undH. Kuckertz, Angew. Chem.75, 95 (1963).Zugleich 2. Mitt. über silylsubstituierte Carbodiimide; 1. Mitt.J. Pump undU. Wannagat, Ann. Chem.652, 21 (1962); Angew. Chem.74, 117 (1962); Österr. Chemiker-Ztg.62, 319 (1961). 相似文献
76.
77.
Harro Lentz Ernst Ulrich Franck 《Angewandte Chemie (International ed. in English)》1978,17(10):728-730
Liquid or dense supercritical ammonia has been suggested as an extraction fluid. It is indeed good solvent for very different classes of compounds, as can be seen from phase diagrams. Such diagrams for binary systems of ammonia and hydrocarbons are presented and discussed on the basis of their critical curves. Apparatus and methods for the measurement of phase equilibria and equation of state data of fluid mixtures at high pressure are described. 相似文献
78.
79.
Klaus Behmel Manfred Schulze und Ulrich Annagat 《Fresenius' Journal of Analytical Chemistry》1968,241(1):1-4
Zusammenfassung Eine einfache und genaue Methode zur Bestimmung von Si-H- und Si-Si-Gruppen wird vorgeschlagen, die auf alkalischer Hydrolyse der Substanz in einem verschlossenen und evakuierten Kolben und AuswÄgen des dem entwickelten Wasserstoff entsprechenden Wasservolumens beruht. Bei H-Gehalten von 1–2% betrÄgt die Genauigkeit ± 0,03% (abs.).
Herrn Prof. Dr. E. Asmus zum 60. Geburtstag gewidmet. 相似文献
Note on the quantitative determination of Si-H- and Si-Si-groups
A simple, robust and surprisingly exact method for the quantitative determination of Si-H- or Si-Si-groups is based on alkaline hydrolysis of the Si-H- or Si-Si-containing substances in a sealed and evacuated vessel and weighing of the volume of water equivalent to the developed volume of hydrogen. The accuracy is ± 0.03% (abs.) with H contents of 1–2%.
Herrn Prof. Dr. E. Asmus zum 60. Geburtstag gewidmet. 相似文献
80.