The 60 MHz1H NMR spectra of racemic ketazolam, 1, have been studied at 28° in CDCl3solution with the achiral reagent tris(6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedionato)europium(III), 2 and the chiral reagent tris[3-(heptafluoropropylhydroxymethyl- ene)-d-camphoratoleuropium(III),3. Dramatic differences in lanthanide-induced shifts,Δδ, were observed for the diastereotopic CH2protons with either added2or1. Differences in these Δδ valuest as well as differences in lanthanide-induced line broadening and in enantiomeric shift differences (observed with3) are interpreted in terms of a relatively rigid preferred conformation of1. Assignments for the CH2protons are made. Direct optical purity determinations for samples oflshould be possible by use of3, based on resonances for either of the CH2protons or the allylic CH3.