The core bicyclo[7.3.0]enediyne 3 has been synthesized from the protected cyclohexane-1,2-dione 6 and enediyne component 9. Conversion of 20 into more highly functionalized enediynes was accomplished by oxidation and amination to give 27. Protection of 27, and conversion into 31, gave on treatment with (MeO)(2)P(O)CH2CO2Me the lactone 32, which was transformed into the trisulfide 39. All attempts to deprotect 39, using conditions that other workers successfully applied to similar substrates, only resulted in the cyclic sulfides 42 and 43.