The alkylation of malonate derivatives with the new bis-electrophile 4
gave 18-membered macrocyclic enediynes 6a-c by a 2:2 alkylation proce
ss. The thermal stability of the bis(enediyne) 6a was investigated by
differential scanning calorimetry. X-ray structure analyses revealed c
hair and twisted conformations of the macrocycles 6b and 6c in the cry
stal.