Transients from a mixture of [(R(O)Sn)2C(CH3)2]2 and (RCl2Sn)2C(CH3)2 [R = (SiMe3)2CH]: an identification in situ by 1D 119Sn and 2D 1H119Sn HMQC NMR spectroscopy and electrospray mass spectrometry

✍ Scribed by Monique Biesemans; Andrew Duthie; Klaus Jurkschat; Ingrid Verbruggen; Rudolph Willem; Bernhard Zobel

• Publisher: John Wiley and Sons
• Year: 2003
• Tongue: English
• Weight: 147 KB
• Volume: 17
• Category: Article
• ISSN: 0268-2605
• DOI: 10.1002/aoc.443

✦ Synopsis

The reaction of the 2,2-bis(organodichlorostannyl)propane [(Me 3 Si) 2 CH(Cl 2 )Sn] 2 CMe 2 (A) with the corresponding organotin oxide {[(Me 3 Si) 2 CH(O)Sn] 2 CMe 2 } 2 (B) does not provide the corresponding normally expected tetraorganodistannoxane {[(Me 3 Si) 2 CH(Cl)SnCMe 2 Sn(Cl)CH(SiMe 3 ) 2 ]O} n but a complex reaction mixture. One major product, namely the 2,4,6,8-tetraorgano-2,6-dichloro-1,5,9trioxa-2,4,6,8-tetrastannabicyclo[3.3.1]nonane derivative [(Me 3 Si) 2 CHSnCMe 2 Sn(Cl)CH(SiMe 3 ) 2 ] 2 O 3 (C) was identified in situ by 2D 1 H-119 Sn and 1 H-13 C heteronuclear multiple quantum coherence and heteronuclear multiple bond correlation NMR spectroscopy as well as electrospray mass spectrometry. Compound C is proposed to be in equilibrium with an ionic species C , the cation of which has an adamantane-type structure.