Duff反应法合成5-壬基水杨醛

5-壬基水杨醛是合成5-壬基水杨醛肟的重要中间体，5-壬基水杨醛肟作为铜萃取剂在工业上有很多应用。以4-壬基酚、六次甲基四胺为原料，醋酸为溶剂，经Duff反应合成了5-壬基水杨醛。相对其他合成5-壬基水杨醛的方法，采用Duff反应来合成具有操作简便、反应周期较短、产物单一且容易进行提纯等优点。通过对原料的物质的量之比、反应时间、反应温度等因素对目标产物收率的影响，确定了合成5-壬基水杨醛适宜的反应条件：n(4-壬基酚)∶n(六次甲基四胺)=1∶2，反应温度为90 ℃，醋酸为溶剂，反应6 h。在上述条件下，以4-壬基酚计，目标产物的收率为98.7%，液相色谱纯度为92.0%，产物经¹H-NMR表征，其结构目标产物一致。

Synthesis of 5-Nonylsalicyaldehyde by Duff Reaction

5-Nonylsalicylaldehyde was the important intermediates in the synthesis of 5-nonylsalicylaldoxime,which as copper extraction agent had many applications in industry.In this paper,5-nonylsalicyaldehyde was synthesized from 4-nonylphenol,hexamethylenetetramine in acetic acid via Duff reaction.Compared to the other synthesis methods,the synthesis method of 5-nonylsalicyaddehyde used Duff reaction has much advantages,such as simple operation,short reaction period,single product and easy to be purified.The effects of reactant mole ratio,reaction temperature,reaction time on the reaction yield were studied.The optimum reaction conditions were as follows： n（4-nonylphenol） ∶ n（hexamethylenetetramine） = 1∶ 2 and the reaction mixture was dissolved in acetic acid and stirred at 90 ℃ for about 6 h.Under these conditions,the yield of 5-nonylsalicyaldehyde was 98.7% based on 4-nonylphenol with a purity of 92.0%（analyzed by HPLC）.Structure of the product was elucidated by1H-NMR analysis.