CHEMIE POLYFUNKTIONELLER LIGANDEN. LXXIII. SYNTHESE, STRUKTUR UND REAKTIONSVERHALTEN VON CRYPTANDEN (BZW. SPHERANDEN) MIT DEN HETEROELEMENTEN ARSEN, SAUERSTOFF, SCHWEFEL UND STICKSTOFF

Article abstract of DOI:10.1016/0022-328X(83)80079-5

The reaction of N(CH2CH2Cl)3 (I) with KAs(C6H5)2*dioxane (1/2) in THF yields, as Sacconi et al. reported earlier, 80percent of N3 (II).II is now obtained in a still higher quantity from the reaction of Cl (III) with NaAs(C6H5)2 in liquid ammonia.Treatment of II with gaseous HI in dry CH2Cl2 results in the formation of I (IV), which is isolated by recrystallisation from THF as I*THF (1/1) (IVa).IVa reacts with H2O/NH3 or H2S/N(C2H5)3 to give the novel cryptands 8(As4O4)6 (V) or 8(As4S4)6 (VI), which also can be denoted as spherands.The reaction of V with dry gaseous HCl in benzene leads to Cl (VII).All the new compounds are characterized, as far as possible, by their IR, FIR, Raman, 1H NMR and mass spectra.To determine the structure of V a single X-ray crystal study was carried out.Moreover II, which is already well-known but not completely characterized, is included in this discussion only for spectroscopic comparison.