A series of optically pure 3, 3′-bis (RO)-MeO-BIPHEP derivatives are prepared and used in palladium catalyzed asymmetric transformations. The phosphine oxide of is prepared in four steps from p-methoxyphenol and resolved using the novel resolving reagent chloro (l- menthoxy) dimethylsilane. Subsequent conversions provide catalysts and. Ligands, and are prepared in six steps from p-methoxyphenol and the phosphine oxides of and, and are ...