Beiträge zur Chemie des Sulfamids, 1. Mitt.: Zur Konstitution des Disilber-sulfamids

According to spectroscopic (IR, broadline proton NMR) and chemical (alkylation) investigations of disilver sulphamide the following molecular structure is assumed: $$\begin{gathered} O \hfill \\ || \hfill \\ H_2 N\_\_S\_\_NAg| \hfill \\ OAg \hfill \\ \end{gathered}$$ From the IR and NMR data deduction concerning the nature of the chemical bonds in this compound is possible. The instability of the still unknown mono-and trisilver sulphamide is discussed with regard to the structure of disilver sulphamide.     

Improved flask-combustion method for phosphorus in petroleum products

Summary An electrical assembly for the oxygen-flask combustion of lubricants and similar petroleum products is described. The pyrolysis is performed in two consecutive steps. After the ignition and burning of the sample (sorbed on sodium carbonate) the combustion is completed by further heating. The sample weight should not exceed 140 mg. In this way the sensitivity of phosphorus determination of the tentative IP standard procedure is enhanced from 0.01 to 0.001% phosphorus if the volume of solution for the final spectrophotometric measurement is reduced.

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Zusammenfassung Ein elektrisches Gerät für die Verbrennung von Schmierölen und ähnlichen Erdölprodukten im Schöniger-Kolben wurde beschrieben. Die Pyrolyse erfolgt in zwei aufeinander folgenden Schritten. Nach der Entflammung der an Natriumcarbonat adsorbierten Probe und nach Erlöschen der Flamme erfolgt die vollständige Verbrennung von Einwaagen, die 140 mg nicht überschreiten. So konnte die Empfindlichkeit der Phosphorbestimmung nach der tentativen IP-Standardmethode von 0,01% auf 0,001% Phosphor gesteigert werden, wenn man die spektrophotometrische Messung mit vermindertem Lösungsvolumen durchführt.

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Herrn Professor Dr. H. Lieb zum 90. Geburtstag gewidmet.     

Synthesis of (4S,9aS)-hexahydro-4-methyl-1H,5H-pyrrolo[2,1-c][1,4]-thiazepine-1,5-dione,A potent angiotensin converting enzyme inhibitor

Synthesis of (4S,9aS)-hexahydro-4-methyl-1H,5H-pyrrolo[2,1-c][1,4]thiazepine-1,5-dione, an orally active potent angiotensin converting enzyme inhibitor is described.     

Bound states and scattering resonances of OH(A)-He

The OH-He complex has been observed using laser excitation of the A 2sigma+-X 2pi transition. The bands of the complex were close to the monomer rotational lines that terminate on the n = 0, 1, and 2 levels of OH(A). The unresolved band associated with He.OH (A,n=0) was redshifted from the OH parent line by 1.6 cm(-1), providing a direct measurement of D0'-D0". The complex features associated with n = 1 and 2 were identified as scattering resonances. They have been assigned by comparison with resonance structures derived from close-coupling calculations. The ab initio potential energy surface of H.-S. Lee, A.B. McCoy, R.R. Toczylowski, and S.M. Cybulski, [J. Chem. Phys. 113, 5736 (2000)] was used in these calculations. The level of agreement between the observed and predicted resonances indicated that the ab initio surface is reasonably accurate.     

Beiträge zur Chemie der Alkylverbindungen von Übergangsmetallen. XLIV. Tetrakis(alkoxycarbonylmethyl)titan-Verbindungen

Contributions to the Chemistry of Transition Metal Alkyl Compounds. XLIII. Tetrakis(alkoxycarbonylmethyl)titanium Compounds Organotitanium(IV) compounds of the type (ROCOCH₂)₄Ti (R ? C₂H₅, i-C₃H₇, t-C₄H₉, C₆H₅, C₆H₅CH₂) were obtained by reactions of ROCOCH₂Li derivatives with TiCl₄ at low temperature. The compounds which decompose only above 90°C were characterized by the hydrolysis products, anaerobic reactions with iodine, and the i.r. spectra. The bond conditions are discussed.     

On the determination of polarity parameters of silica by means of solvatochromic probe dyes

Empirical solvent parameters of silica surfaces are determined by means of solvatochromic dyes, e.g., Cu(tmen) (acac)⁺ ClO ₄ ^– /B(C₆H₅) ₄ ^– , Fe(phen)₂(CN)₂, and Michlers Ketone dissolved in 1,2-dichloroethane or cyclohexane. The values obtained by UV/VIS-measurements are compared with both the polarity scales of Kamlet and Taft and with Gutmann's donor and acceptor numbers. Kamlet and Taft's -parameter (the hydrogen-bond donation capacity of a solvent) is determined independently by means of salicylideneaniline. The ^* of silica is determined using 5-N,N-dimethylamino-5-nitro-2,2-bithiophene and the complex of tetracyanoethylene with Michlers Ketone, respectively. Further on the reliabilities of the obtained Kamlet-Taft parameters , , and ^* are checked by comparism with experimental and calculated values of theE _T(30)-parameter of silica by means of multi-parameter regression analysis. The surface properties of silica are influenced mainly by HBD-properties (75%) and dipolarity/polarizability ^* (20%), but hardly by the HBA-properties (<5%). UV/VIS-measurements were carried out in a special equipment with glass fiber optics, A drawing of the apparatus is given.     

Die Strommer-Zykliden des Flaggenraumes

According to H. BRAUNER a flag space is a three-dimensional affine space with an absolute {,f,F}, wheref is a line in the plane of infinity andF a point onf. A cyclide is a surface of order 4 that intersects only atf. A STROMMER-cyclide is a cyclide generated by translation of a circle in an isotropic plane. In this paper we proof that all STROMMER-cyclides can be generated by translation of an isotropic circle along a divergent Newton-parabola or a conic in a full isotropic plane. We give normal-forms and CAD-pictures of these surfaces. Finaly some geometrical results about STROMMER-cyclides are developed.

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Herrn o.Prof. Dr. Gy. Strommer zum 70. Geburtstag gewidmet.