相转移催化合成2,2-二羟甲基丙酸(DMPA)的研究

Synthesis of 2,2-dimethylolbutyric acid

以甲醛和丙醛为原料,在相转移催化作用下经羟醛缩合及氧化反应合成了2,2一二羟甲基丙酸(DMBA)。缩合反应在30℃,n(甲醛)/n(丙醛)=2.2,催化剂为十六烷基三甲基溴化铵(HDTMA),用Na2CO3和Na0H的混合碱调pH=9,反应2h。反应后立即加盐酸中和调pH=5;氧化反应在70℃、反应时间2.5h。反应产物的结构用红外光谱(IR)表征。

Using phase transfer catalyst, 2, 2-dimethylolbutyric acid was prepared and oxidation from formaldehyde and propionaldehyde. The most suitable technological condensation were as follows： phase transfer catalyst was HDTMAB; molar ratio by the aldol condensation conditions for the aldol n （formaldehyde） ： n （propionaldehyde）=2.2：1; pH=10;reaction temperature 30℃, and reaction time 2.0 h. The most suitable technological conditions for the oxidation were as follows： pH =4; reaction temperature 70℃, and reaction time 2.5h.The product structure was identified by FT-IR.