Abstract In order to synthesize rose oxide (Ⅰ), three step reactions were used, which involved oxidationreduction reaction and cyclization. In the first two steps, the 3,7-dimethyl-oct-5-en-1,7-di-ol (Ⅱ) and 3,7-dimethyl-oct-7-en-1,6-diol (Ⅲ) are synthesized from β-citronellol. Finally, the rose oxide (Ⅰ) was cyclized from Ⅱ and Ⅲ with acidic catalysts. Dosage of hydrogen peroxide, molar ratio, type and dosage of catalyst and reaction time were optimized. Under the optimized conditions, the yields of mixed diols (Ⅱ and Ⅲ) and rose oxide (Ⅰ) are 95% and 41.5% respectively, and the total yield is 39.4%.