Aluminum sec-butoxide was synthesized from aluminum foil and alcohol. The characteristics of the alumina powder prepared from the synthesized alkoxide by the Yoldas method were studied. As a result of measuring the synthesized aluminum sec-butoxide by GC, the purity of the synthesized alkoxide was 98.7% on the basis of commercial alkoxide and the yield was 78.5%. A127-MASNMR analysis shows that powders dried at 9$0^{\circ}C$ and $\alpha$-Al2O3 have 6-cordinated structure and ${\gamma}$-Al2O3 has 4-coordinated structure. The characteristics of alumina powder prepared from the synthisized alkoxide showed the same characteristics with the alumina powder prepared from the commercial alkoxide.