129Xe on Ir(111): NMR study of xenon on a metal single crystal surface.

NMR experiments of (129)Xe adsorbed on an iridium single crystal surface are reported. Very high nuclear polarization (P(z) approximately 0.7) makes the experiment possible. A coverage of less then one monolayer is investigated on the Ir(111) surface with an area of 0.8 cm(2). The observed resonance line shifts are very large and highly anisotropic. We find sigma(iso) = 1,032 +/- 11 ppm and sigma(an) = 291 +/- 33 ppm, which are far above the typical range of physisorption. The highly ordered substrate leads to homogeneous conditions for the xenon atoms, as seen in the narrow linewidth of 20 ppm. Chemical shifts under physisorption conditions are not large enough to totally explain the results. Knight shift can clearly be identified as the cause of the findings. This shift shows the presence of conduction electrons of the metallic substrate at the xenon nucleus and thus the mixing of metallic and atomic states at the Fermi level. Such mixing is in accordance with recent Hartree-Fock and density functional calculations of similar van der Waals adsorption systems. Quantitative comparisons, however, fail completely. The size and ratio of sigma(an) and sigma(iso) are pure ground-state properties in a structurally simple system. They are accessible to theory and provide detailed local information that can serve as a benchmark for theory.

Particle detected Fourier transform NMR at single crystal surfaces--6Li on Ru(001).

Fourier transform nuclear magnetic resonance at single crystal surfaces is described. The adsorption of 6Li on Ru(001) is investigated by newly developed techniques utilizing atomic beam sample preparation and optical detection of the NMR signal on desorbing atoms (laser induced fluorescence) or ions (beamfoil spectroscopy). In complete analogy to magnetically detected NMR, the transverse magnetisation is coherently recorded. This allows pulse NMR to be applied to surface problems.

[Potential cardiotonics. 15. Crystal modifications of 3-cyano-2-morpholino-5-(4-pyridinyl)pyridine (AWD 122-14)]. / Potentielle Kardiotonika. 15. Mitteilung: Kristallmodifikationen von 3-Cyan-2-morpholino-5-(pyrid-4-yl)pyridin (AWD 122-14).

The preparation and X-ray crystallographic characterisation of 10 polymorphic or pseudo-polymorphic forms of the novel cardiotonic AWD 122-14 are described. Thermic transformations of some polymorphic forms into the alpha-form was proved by thermogravimetric analysis and powder diffraction pattern. In dissolution behaviour no significant differences were found between the crystalline modifications but with regard to galenic processing compact alpha-, gamma- and epsilon-forms show advantages.

[Crystal modifications of 3-cyan-6-methyl-5-(pyrid-4-yl)-1,2-dihydropyrid-2-one (milrinone)]. / Kristallmodifikationen von 3-Cyan-6-methyl-5-(pyrid-4-yl)-1,2-dihydropyrid-2-on (Milrinon).

The preparation and characterisation of crystalline alpha-, beta- and gamma modifications of 3-cyan-6-methyl-5-(4-pyrid-4-yl)-1,2-dihydropyrid-2-on e are described. The thermic transformation of alpha- and beta-modification into gamma-modification was proved by thermogravimetric analysis (t.g.a.), differential scanning calorimetry (d.s.c.), IR and powder diffraction pattern. In dissolution behaviour no significant differences were found between the modifications.

[The synthesis of 3-amino-5-(4-pyridinyl)-1,2-dihydropyrid-2-one (Cordemcura) from a technical mixture of pyridines]. / Untersuchungen zur Synthese von 3-Amino-5-(pyrid-4-yl)-1,2-dihydro-pyrid-2-on (Cordemcura) aus technischen Pyridinbasengemischen.

For preclinical and clinical research the headline compound 6 has been synthesized from pyrid-4-yl-malondialdehyde (3) and its bis-N,N-dimethyl)-aldimin-derivative 1 by cyclization with cyanoacetamide giving 4, partial hydrolysis to the amide 5, and degradation by sodiumhypochlorite to the amine 6, concerning to the way described in patent literature. Starting product was a mixture of alkyl pyridines from which 4-picoline reacted selectively with the Vilsmeyer-complex of phosgene/DMF to give cristalline 1. Optimization in all steps resulted in a procedure that gives us the intermediates in good yields and qualities and the final product 6 with high purity, suitable for pharmaceutical use.