2_2_二羟甲基丁酸的合成.pdf

11 585 2, 2- 1 2 , ( 1. , 453003; 2. , 100091) : 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, 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10 mL 时, 在15 °C反应5 h, 2, 2-二羟甲基丁醛的最高摩尔收率可达到58. 5% ; 然后 加入 180 溶剂( 水) 和64 过氧化氢, 在70°反应8 , 2, 2-二羟甲基丁酸的最高摩尔收率为 mL mL C h 66. 0% 。用红外光谱和核磁共振证明了该化合物的结构。 : 2, 2-二羟甲基丁醛; 2, 2-二羟甲基丁酸; 醛醇缩合; 氧化 + : O 621 3 6: A : 0367-6358( 2003) 11-0585-03 Pre arat ion of 2,2-Dimethylolbutyric Acid - 1, - 2 LI Cai yun LI Gai yun ( 1. Dep artment of Chemistry Engineering Pingy uan Univerisity , H enan X inxiang 453003, China; 2. esearch I nstitute of Wood I ndustry , ChineseA cademy of Forestry , Beij ing 100091, China) Abstract: Using inorganic base as a catalyst, 2, 2-dimethylolbutyraldehyde w as re ared by aldol condensa- tion from formaldehyde and butyraldehyde. T aking hydrogen eroxide as an oxidant, 2, 2-dimethylolbu- tyraldehyde w as oxidized further. As a w hite crystal, 2, 2-dimethylolbutyric acid was obtained under cool- , . , , , ing and then urified by recrystallization The reaction conditions including molar ratio reaction time solvent, reaction tem erature and so on w ere investigated. When 2. 2 mol formaldehyde, 1 mol butyralde- hyde and 10 mL 10% aqueous sodium hydroxide reacted at 15 C for 5 h, the molar yield of 58. 5% for 2, 2-