We describe the efficient preparation of Bippyphos, 1. The key precursor to Bippyphos, 5, was prepared via a one-pot bromination of diketone 2 followed by alkylation with pyrazole and condensation with phenylhydrazine. Lithiation of 5 and trapping with di-tert- butylchlorophosphine afforded Bippyphos, 1. Using this approach we have prepared several derivatives of Bippyphos to probe the structure and activity relationships of this family of ...