2,2-二羟甲基丁酸的合成

在碱性催化剂的存在下,甲醛和丁醛进行羟醛缩合反应,制备2,2-二羟甲基丁醛。再以过氧化氢为氧化剂,通过氧化,结晶,重结晶,得到2,2-二羟甲基丁酸的白色晶体。研究了原料摩尔比、反应温度、反应时间、溶剂等反应参数的影响。当甲醛与丁醛的摩尔比为2.2∶1,催化剂(10%NaOH)用量为10mL时,在15°C反应5h,2,2-二羟甲基丁醛的最高摩尔收率可达到58.5%;然后加入180mL溶剂(水)和64mL过氧化氢,在70°C反应8h,2,2-二羟甲基丁酸的最高摩尔收率为66.0%。用红外光谱和核磁共振证明了该化合物的结构。

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.