An efficient and reliable procedure for the preparation of dirhodium(II) tetrakis[ N -phthaloyl-( S )- tert -leucinate], Rh2( S -PTTL)4, a universally effective catalyst for a range of enantioselective carbene transformations, is described. The N -phthaloylation of ( S )- tert -leucine by the method of Bose with essentially no racemization is a key to this process.