Optically pure bisphosphine oxides were conveniently synthesized by Kolbe e
lectrolytic coupling reaction of carboxylic acids possessing a chiral phosp
hinoyl group in 60-65% isolated yield. This synthetic approach provides a v
ariety of accesses to P-chiral bisphosphine ligands. Their absolute configu
rations were intercorrelated with that of the previous reported BisP*-boran
e. Asymmetric hydrogenation of alpha-(acylamino)acrylic acids by a rhodium
complex with BisP* (R = t-octyl or 1,1,3,3-tetramethylbutyl) affords N-acyl
amino acids in 94-96% ee.