Preparation Of 2, 2-Dimethylolbutyric Acid

Using inorganic base as a catalyst, 2,2-dimethylolbutyraldehyde is prepared by aldol condensation from formaldehyde and butyraldehyde. Taking hydrogen peroxide as an oxidant, 2,2-dimethylolbutyric acid is oxidized further. As a white crystal 2,2-dimethylolbutyric acid is obtained under cooling, and then purified by recrystallization.As for the aldol condensation, the technical conditions, including reaction time, reaction temperature, molar ratio and so on, have been examined. Based on the added amount of butyraldehyde, the molar yield of 58.6% for 2,2-dimethylolbutyraldehyde was attained. All data about the kinetic process were acquired from packed or capillary GC.With respect to the oxidation, the various reaction conditions, including molar ratio, reaction time, solvent, and reaction temperature, have been investigated. By the added amount of 2,2-dimethylolbutyraldehyde, the molar yield of 66.0% for 2,2-dimethylolbutyric acid was accomplished. HPLC was used for analyzing the chemical composition of reaction mixtures in the oxidation.The structure of the aimed compound was confirmed by IR and NMR, and the purity is the same as one made by NKC.