摘要
以4-壬基酚、镁和多聚甲醛为原料,甲苯为溶剂,经甲酰化反应合成了5-壬基水杨醛.通过对关键因素的考察,得到合成5-壬基水杨醛的较优条件为:甲醇∶镁=10∶1,4-壬基酚∶镁∶多聚甲醛=1∶0.6∶2.6,多聚甲醛投料温度为95~100℃,之后再保温100~110℃反应2 h.在上述条件下,以4-壬基酚计,目标产物的收率为93.7%,液相色谱纯度为98.2%,产物经1H-NMR表征与目标产品一致.
5-nonylsalicyaldehyde was synthesized from 4-nonylphenol, magnesium scraps and paraformaldehyde in toluene by formylation. By studying the crucial factors the optimal conditions were obtained as follows: n(methanol) : n(magnesium) = 10 : 1, n(4-nonylphenol) : n(magnesium) : n(paraformaldehyde)= 1 : 0.6 : 2.6, paraformaldehyde was charged at 95 - 100℃, and the reaction mixture was stirred at 100 - 110℃ for about 2 h. Under these conditions, the yield of 5-nonylsalicyaldehyde was 93.7% based on 4-nonylphenol with a purity of 98.7% (analyzed by HPLC). The structure of the product was elucidated by 1H-NMR analysis.
出处
《河北工业大学学报》
CAS
北大核心
2011年第5期62-65,共4页
Journal of Hebei University of Technology
关键词
5-壬基水杨醛
4-壬基酚
甲酰化
多聚甲醛
镁
5-nonylsalicylaldehyde
4-nonylphenol
formylation
paraformaldehyde
magnesium