Preparation of 2,2-Dimethylolbutyric Acid

Using inorganic base as a catalyst, 2,2dimethylolbutyraldehyde was prepared by aldol condensation from formaldehyde and butyraldehyde. Taking hydrogen peroxide as an oxidant, 2,2dimethylolbutyraldehyde was oxidized further.As a white crystal, 2,2dimethylolbutyric acid was obtained under cooling, and then purified by recrystallization. The reaction conditions, including molar ratio, reaction time, solvent, reaction temperature and so on were investigated. When 2.2 mol formaldehyde, 1 mol butyraldehyde and 10 mL 10% aqueous sodium hydroxide reacted at 15°C for 5 h, the molar yield of 58.5% for 2,2dimethylolbutyraldehyde was attained. Then by adding 180 mL solvent (water) and 64 mL peroxide, the oxidation reaction was conducted at 70°C for 8 h. The molar yield of 66.0% for 2,2dimethylolbutyric acid was accomplished. The structure of the aimed compound was confirmed by IR and NMR.