5-壬基水杨醛肟的合成

SYNTHESIS OF 5-NONYLSALICYALDEHYDE OXIME

以4-壬基酚、多聚甲醛和盐酸羟胺为原料,经甲酰化和肟化2步反应合成了5-壬基水杨醛肟,其适宜的反应条件为:1)甲酰化反应,n(4-壬基酚):n(镁):n(多聚甲醛)=1:0.59:(3～4),保温时间以2 h为宜;2)肟化反应,n(4-壬基酚):n(盐酸羟胺)=1;1.15,以4-壬基酚计的产物收率为97.5%,液相色谱纯度为95.1%。产物结构经MS和^(13)C NMR分析确定。与文献方法相比,收率提高了7%以上。

5-Nonylsalicyaldehydeoxime was prepared from 4-nonylphenol, paraformaldehyde and hydroxylamine hydrochloride by formylation and oximation. The optimal conditions were found as follows, in formylation reaction, n （4-nonylphenol） ： n （magnesium） ： n （paraformaldehyde） = 1： 0.59 ：（3 - 4）, reaction time 2 h; in oximation reaction, n（4-nonylphenol） ： n（hydroxylamine hydrochloride）=1 ： 1.15. Under these conditions, the yield of the desired product reached 97.5% （based on 4-nonylphenol） with 95.1% purity （determined by HPLC）. The structure was elucidated by MS and ^13C NMR analysis. Comparing to the literature methods, the yield was increased by 7%.