Cyclodi(chenodeoxycholate) dipentenoate was synthesized by Yamaguchi macrolactonization by adding 2,6-dichlorobenzoyl chloride pre-reacted with 4-pentenoic acid and p-dimethylaminopyridine (DMAP) to chenodeoxycholic acid (CDCA). Nice crystals of this compound were obtained. Another main compound, 3á,7á-bis(4-pentenoyloxy)-24-cholanoic acid was also obtained. The structures of these compounds were characterized by NMR and FAB mass spectrometry. The potential application of cyclocholates based on CDCA and CA in biological field has a lot of promise.