The skeletal isomerization of 3,3-dimethyl-l-butene over AIPO4 (AI/P=I), CrPO4 (Cr/P=I), and CrPO4-AIPO4 (CrAIP, 5-10 wt.% A1PO4) catalysts is a first order reaction. Catalytic performance is affected by the precipitation agent. CrPO4 catalysts obtained in propylene oxide-aqueous ammonia showed the highest activity. Moreover, the incorporation of AIPO4 to CrPO4 developed CrAlP catalysts that exhibited increased activity, irrespective of the precipitation method, as compared with both A1PO4 and CrPO4 catalysts. Besides, CrAIP catalysts prepared in propylene oxide-aqueous ammonia were the more active ones.