In this research, heterobimetallic palladium-cobalt acetate was used as catalyst for the intramolecular carbon - carbon π bond nitrene insertion reaction. Allyl and homoallyl alcohols were used as starting material to synthesis allyl sulfamate and homoallyl sulfamate. PdCo(OAc)4 was found capable of catalyzing the nitrene insertion and the desired bicyclic aziridine compounds were obtained. Five and seven-membered ring compounds were also observed via ring opening of the aziridines by acetate. During the optimization of the reaction conditions, PdCo(OAc)4 made from different brands of palladium acetate, resulted different yield in the catalyzed aziridination reaction.