A study directed at the enantioselective synthesis of spirodiketopiperazine homologues of hydantocidin is described. Furanoid glycals, systems that are amenable to C-5 metalation in the presence of tert-butyllithium, are readily coupled to N-protected 2, 3-azetidinediones provided that at least 1 equiv of BF3⊙ OEt2 is present to curb enolization. The resulting 1: 1 mixtures of carbinols undergo smooth ring expansion to spirocyclic keto amides when ...