在Na_2HPO_4-NaH_2PO_4缓冲溶液中催化合成2,2-二羟甲基丁酸(DMBA)

Synthesis of 2,2-dimethylolbutyric acid(DMBA)base in H_2PO^-_4-HPO^(2-)_4 buffer solution

在Na2HPO4-NaH2PO4缓冲溶液中以甲醛和丁醛为原料,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:在Na2HPO4-NaH2PO4缓冲溶液中调pH约为11,反应温度为30℃,n甲醛∶n丁醛=2.2∶1,反应时间为2.5h;2,2-二羟甲基丁醛氧化反应的最佳工艺条件为:nH2O2∶n丁醛=1.1∶1,溶液的pH约为4,反应温度为70℃,反应时间为2h。反应产物的结构用红外光谱(IR)表征。

H2PO4^- -HPO4^2- buffer solution, 2,2-dimethylolbutyric acid was synthesized by the mixed aldol condensation and oxidation from formaldehyde and butyraldehyde. The most suitable technological conditions for the aldol condensation were as follows ： pH ≈ 11 ; molar ratio n （ formaldehyde ） ： n （butyraldehyde） = 2.2： 1 ;reaction temperature 30℃ and reaction time 2.5h. The most suitable technological conditions for the oxidation were as follows： n （H202） ： n （butyraldehyde） = 1.1 ： 1 ; pH ≈ 4 ; reaction temperature 70℃ and reaction time 2h. The structure of the product was confirmed by IR.