Catalyzed synthesis of 3-methylbut-3-en-1-ol acetate and its hydrolysis

Anchoring of tin dichloride on quaternary ammonium chloride functionalized MCM-48 as a new catalyst was used to catalyze the condensation reaction of paraformaldehyde, isobutene and acetic acid to produce 3-methylbut-3-en-1-ol acetate. By using the innovative esterification-hydrolysis two-step method, 3-methylbut-3-en-1-ol was synthesized effectively. The process conditions of esterification reaction and hydrolysis reaction were investigated. The result shows that under the optimal esterification reaction condition of 2.4 g catalyst, 16 g paraformaldehyde, 120 g isobutene, 128 g acetic acid, reaction temperature 140°C, reaction time 6 h, the yields of 3-methylbut-3-en-1-ol acetate and 3-methylbut-3-en-1-ol are 55.5% and 13.8%. The yield of hydrolysis is 94.5% under the optimal reaction condition of reaction temperature 50°C, mass fraction of alkali solution 20%, feed rate of alkali solution 20 mL/h. The final yield of MOH prepared by esterification-hydrolysis two-step method reaches to 65.5%.