2,2-二羟甲基庚醛的合成与表征

以甲醛和新蒸庚醛为原料,经羟醛缩合反应合成了2,2-二羟甲基庚醛(DMH)。羟醛缩合反应的最佳工艺条件为:反应温度为35℃,n(甲醛)∶n(庚醛)∶n(NaOH)=4∶1∶1.3,缩合剂为w(NaOH)=10%溶液,反应时间为5 h。加甲酸中和碱,经精制DMH的收率达到67.8%。2,2-二羟甲基庚醛的结构用红外光谱(IR)、1H和13C核磁共振谱表征。

Synthesis and characterization of 2,2-dimethylolheptaldehyde

2,2-Dimethylolheptaldehyde was prepared from formaldehyde and n-heptaldehyde through condensation reaction.The optimum conditions of condensation reaction were as follows:temperature 35 ℃,reaction time 5 h and molar ratio n(formaldehyde) ∶n(n-heptaldehyde) ∶n(sodium hydroxide)=4 ∶1 ∶1.3 with w(sodium hydroxide sulution)=10% as catalyst.Through neutralization by adding formic acid,2,2-dimethylolheptaldehyde was purified and its mass content reached 67.8%.The structure of the product was confirmed by IR,1H and 13C NMR spectrum.