It was found that Pt/SbOx catalysts were active for the selective oxidation of i.C4H10 and i-C4H8 to methacrolein (MAL) at 773 K. The SbOx itself was inactive for the selective oxidation of i-C4H10, while i-C4H8 was converted to MAL on the SbOx. Small amounts of Pt (0.2-0.72 wt%) supported on the SbOx promoted the i-C4H10 oxidation with good selectivity to MAL (typically 50-60%) and MAL + i-C4H8 (80-90%). The selective oxidation of i-C4H8 to MAL was also markedly enhanced by Pt. The performance of Pt/SbOx catalysts for the i-C4H10 selective oxidation may be attributed to combinative catalysis of Pt particles modified with SbOy (y < x) and Sb6O13 produced under the oxidation conditions.