198143-95-2Relevant academic research and scientific papers
Tri(tert-butyl) plumbyl derivatives of group 14 elements: Multinuclear magnetic resonance studies: Determination of coupling signs
Herberhold, Max,Troebs, Volker,Wrackmeyer, Bernd
, p. 391 - 400 (2007/10/03)
A solution of tri(tert-butyl)plumbyl-lithium in THF (2) was prepared by the reaction of hexa(tert-butyl)diplumbane (1) with an excess of lithium. Treatment of this reagent with a variety of Group 14 electrophiles gave tetraorganolead compounds tBu3Pb-R (3, R = Me (a), Et (b), nPr (c), nBu (d), CH2Ph (e), CH2SiMe3 (f)), plumbylsilanes tBu3Pb-SiR12R2 (4, R1 = R2 = Me (a), R1 = Me, R2 = tBu (b), R1 = Me, R2 = SiMe3 (c), R1 = Me, R2 = Ph (d), R1 = R2 = Ph (e)), one plumbylgermane tBu3Pb-GeMe3 (5a), plumbylstannanes tBu3Pb-SnR33 (6, R3 = Me (a), Et (b), nBu (c), tBu (d), Ph (e), 1,1′-ferrocenediyl (f)), and hexaorganodiplumbanes tBu3Pb-PbR43 (7, R4 = Me (a), Et (b), iPr (c), nHex (d), cHex (e)], iPr3Pb-PbEt3 (10) and tBu2(Me)Pb-Pb(Me)tBu2 (11) as a side product. The plumbylstannanes Et3Pb-SnMe3 (9a) and iPr3Pb-SnMe3 (9b) were prepared for comparison of NMR data. All compounds were characterized by 1H, 13C, 29Si, 119Sn and 207Pb NMR data. Signs of coupling constants nJ(207Pb, 13C) (n = 1, 2), 1J(207Pb, 29Si), 1J(207Pb, 119Sn) and 1J(207Pb, 207Pb) were determined by appropriate 1D heteronuclear double resonance experiments and 2D heteronuclear shift correlations. The influence of the tBu3Pb group on the bonding situation is reflected by sign changes of several coupling constants when compared with analogous trimethyllead derivatives.
