相转移催化合成2,2-羟甲基丁酸的研究

Synthesis of 2,2-Dimethylolbutyric Acid with Phase Transfer Catalyst

以甲醛和丁醛为原料,在相转移催化作用下经羟醛缩合及氧化反应合成了2,2-二羟甲基丁酸(DMBA)。羟醛缩合反应的最佳工艺条件为:以十六烷基三甲基溴化铵(HDTMAB)为催化剂用NaOH与碳酸钠混合碱液调pH值约为10,反应温度为30℃,n(甲醛)/n(丁醛)=2.2∶1,反应时间为2 h;2,2-二羟甲基丁醛氧化反应的最佳工艺条件为:n(H2O2)/n(丁醛)=1∶1.1,溶液的pH值约为5,反应温度为70℃,反应时间为2 h。反应产物的结构用红外光谱(IR)表征。

Using phase transfer catalyst, 2, 2-dimethylolbutyraldehyde was synthesised by the aldoi condensation of formaldehyde with butyraldehyde. The optimum reaction conditions for the aldol condensation were as follows： phase transfer catalyst, HDTMAB ; molar ratio n （formaldehyde） ： n （ butyr aldehyde） = 2.2 ： 1 ; The optimum conditions for the oxidation reaction were as follows： n （ H202 ）/n （butyraldehyde） = 1 ： 1.1 ; pH = 5 ; reaction temperature, 70℃ and reaction time, 2h. The structure of the product was confirmed by IR.