Synthesis of (RSn)4X6 Adamantanes (X = O, S, Se) in Liquid Ammonia and in the Two-Phase System Liquid Ammonia/THF

✍ Scribed by Karsten Wraage; Thomas Pape; Regine Herbst-Irmer; Mathias Noltemeyer; Hans-G. Schmidt; Herbert W. Roesky

• Publisher: John Wiley and Sons
• Year: 1999
• Tongue: English
• Weight: 266 KB
• Volume: 1999
• Category: Article
• ISSN: 1434-1948
• DOI: 10.1002/(sici)1099-0682(199905)1999:5<869::aid-ejic869>3.0.co;2-2

✦ Synopsis

The reactions of trisSnBr 3 (1) [tris = (Me 3 Si) 3 C] and nBuSnCl 3 pressure at room temperature results in the formation of (trisSn) 4 S 6 (3) and (trisSn) 4 Se 6 (4). nBuSnCl 3 reacts with Na 2 S with Na 2 X (X = O, S, Se) yield the heterocyclic adamantanes 2-6. The reaction of 1 with Na 2 O is carried out in liquid and Na 2 Se in liquid ammonia at -33 °C under normal pressure to give (nBuSn) 4 S 6 ( 5) and (nBuSn) 4 Se 6 (6), ammonia under normal pressure at -78 °C to give (trisSn) 4 O 6 (2). However, the reaction of 1 with Na 2 S and Na 2 Se under respectively.

gives a singlet at δ ϭ 0.32 for the protons of the methyl

The proton-NMR spectrum of (trisSn) 4 O 6 (2) shows four Compound 1 was characterized by mass spectrometry singlets (δ ϭ 0.13, 0.24, 0.28, 0.51), as does the 29 Si-NMR and NMR-spectral studies. The 1 H-NMR spectrum of 1 spectrum (δ ϭ Ϫ1.0, Ϫ0.42, Ϫ0.27, Ϫ0.17), which indicates that the tris groups are not equivalent. However, the four [a] Institut für Anorganische Chemie der Universität Göttingen, tin atoms are equivalent and the compound gives only one Tammannstraße 4, D-37077 Göttingen, Germany 119 Sn resonance (δ ϭ 94.3). The mass spectrum exhibits the