Structural aspects of the product from glyoxal and tetrakis(ethoxycarbonylamino)ethane

The base-promoted addition of glyoxal to 1,1,2,2-tetrakis(ethoxycarbonylamino)ethane in DMF gives a product mixture containing mostly 1,1′,3,3′-tetrakis(ethoxycarbonyl)-4,4′,5,5,'-tetrahydroxy-2,2′-biimidazolidyl. An alternate structure containing a tetraazadecalin system was considered less likely, since the most significant peak in the mass spectrum of this product and a tetraacetate derivative corresponded to half the mass of the parent ion. Two-dimensional nmr spectra on the major hplc fraction are more consistent with the biimidazolidinyl structure (very low J_vic and lack of NOE enhancement). A HETCOSY spectrum on the mixture allowed assignment of ¹H nmr shifts.     

1,1,3,3,5,5-Hexakis(dimethylamino)-λ5-[1,3,5]triphosphinin – Darstellung,Kristallstruktur und NMR-Daten

1,1,3,3,5,5-Hexakis(dimethylamino)-λ⁵-[1,3,5]triphosphinine – Synthesis, Crystal Structure, and NMR Data Preparation of 1,1,3,3,5,5-hexakis(dimethylamino)-λ⁵-[1,3,5]triphosphinine ( 4 ) and the path of its formation from methyl-bis(dimethylamino)difluorophosphorane ( 1 ) and n-butyllithium are described. The chemical behaviour of compounds of type [R₂P=CH–]_n is compared with that of the isoelectronic dichlorophosphazenes [Cl₂P=N–]_n. The structure of 4 is eludicated by n.m.r. spectra and X-ray structural analysis.     

Electrochemical etching of silicon carbide

Both n- and p-type SiC of different doping levels were electrochemically etched by HF. The etch rate (up to 1.5 μm/min) and the surface morphology of p-type 6H-SiC were sensitive to the applied voltage and the HF concentration. The electrochemical valence of 6.3 ± 0.5 elementary charge per SiC molecule was determined. At p-n junctions (p-type layer on a n-type 6H-SiC substrate) a selective etching of the p-type epilayer could be achieved. For a planar 6H-4H polytype junction (n-type, both polytypes with equal doping concentrations) the 4H region was selectively etched under UV illumination. Thus polytype junctions could be marked by electrochemical etching. With HCl instead of HF no etching of SiC occurs, but a SiO₂ layer (thickness up to 8 μm) is formed by anodic oxidation. Received: 29 October 1998 / Accepted: 27 January 1999     

Die Synthese von 3β-Acetoxy-24-aza-24-desoxa-xysmalogenin,. Partialsynthetische Versuche in der Reihe der Herzgifte. 12. Mitteilung,

Synthesis of 3β-acetoxy-24-aza-24-desoxa-xymalogenin Starting from the pregnenolone-derivative 1 we report the synthesis of the possibly cardiac-active compound 24-aza-24-desoxa-xysmalogenin 15 .     

The Wittig Reaction in Industrial Practice

The effects of a scientific discovery on industrial practice are illustrated with reference to the Wittig reaction. The aim of utilizing the Wittig reaction of linking terpenoid building blocks to give vitamin A and carotenoids on an industrial scale prompted extensive research and development work of a synthetic and chemical engineering nature. The importance of the Wittig reaction and its variants in the synthesis of active compounds and fine chemicals in industrial research is demonstrated in the present article.