Celangulin-V (1) and podophyllotoxin (2) are both natural compounds with significant insecticidal activity. The identical and nonidentical dimers of celangulin-V and podophyllotoxin (3, 4, 5) were synthesized using succinic acid as the linker, and their insecticidal activities against 3rd instar larvae of Mythimna separata were tested. Only the identical dimer of celangulin-V (3) show some insecticidal activity.