Abstract
Treatment of M(dppe)Cl2 (M = Pd, Pt) or Pt((R,R)-Me-DuPhos)Cl2 with IsHPCH2PHIs (1; Is = isityl = 2,4,6-(i-Pr)3C6H2) and 2 equiv of NaOSiMe3 gave the mononuclear diphosphametallacyclobutane complexes M(dppe)(IsPCH2PIs) (M = Pd (2), Pt (3)), or Pt((R,R)-Me-DuPhos)(IsPCH2PIs) (4). Dynamic processes involving phosphorus inversion and rotation about the P–C(Is) bonds in 2–4 were characterized by variable-temperature NMR spectroscopy, which suggested that each existed as a single C2-symmetric diastereomer in solution, consistent with their solid-state structures determined by X-ray crystallography. The MiniPhos derivative IsMePCH2PMeIs (5) was prepared as a 5.5/1 rac/meso mixture by sequential arylation and methylation of Cl2PCH2PCl2. Alternatively, the catalyst precursor Pt((R,R)-Me-DuPhos)(Ph)(Cl) mediated alkylation of secondary phosphines in the presence of NaOSiMe3 to yield selectively meso-5 either from PHMe(Is) and CH2I2 or from 1 and MeI. Recrystallization and chromatography yielded diastereomerically ...
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