Add time:08/04/2019         Source:sciencedirect.com

Reaction of two equivalents of lithium hypersilylphosphanide (hypersilyl, Hyp = tris(trimethylsilyl)silyl) with dichlorotetramethyldisilane at low temperatures gives [HypPH–SiMe2–]2 1, a compound with high steric protection on both phosphane functionalities. Dehydrogenation reaction of 1 with n-butyl lithium yields the dilithiated [2.1.1] bicyclic phosphanide salt [HypPLi–SiMe2–]2 2. The bicyclic structure is confirmed by NMR spectroscopy and X-ray diffraction analysis. As a major byproduct during the synthesis of 1 as well as via reaction of 2 with dichlorotetramethyldisilane, 1,4-diphospha-cyclosilahexane [HypP–(SiMe2)2–]2 3 is obtained. X-Ray diffraction analysis shows exclusive formation of the trans-conformer 3a in the solid state, which is supported by calculations at the level of density functional theory (DFT).

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