Abstract: An ultrasound-promoted method to stable acyclic aliphatic solid enols was developed, which could be finished within 1 h at room temperature with the yields up to 99%, using azo compounds and β-carbyl esters as raw materials by the exploration of catalyst type, reaction temperature, reaction time, ultrasonic reaction conditions on the yields. The adopted reaction had the characteristics of mild conditions, short time, high yield and high product stability. It provided a convenient way for the synthesis of enols. By the method, a series of non-cyclic solid enols were efficiently prepared, and the yield was up to 99%.