摘要
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.
出处
《化学试剂》
CAS
CSCD
北大核心
2005年第11期684-686,共3页
Chemical Reagents