Diisobutyl aluminum chloride is synthesized by the reaction of triisobutyl aluminum and carbon tetrachloride. Diisobutyl aluminum azide (DBAA) is synthesized by the reaction of the sodium azide and diisobutyl aluminum chloride in arenes, and its complex(DBAA·THF) is also synthesized through the reaction of the sodium azide and diisobutyl aluminum chloride in tetrahydrofuran. DBAA and DBAA·THF are characterized by IR and HNMR spectrum. The properties of DBAA and DBAA·THF are also studied.