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5-壬基水杨醛肟的合成
引用本文:李效军,王凯,陈炜,冯成,李春英.5-壬基水杨醛肟的合成[J].精细石油化工,2007,24(3):57-59.
作者姓名:李效军  王凯  陈炜  冯成  李春英
作者单位:河北工业大学化工学院,天津,300130
摘    要: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。

关 键 词:5-壬基水杨醛肟  4-壬基酚  甲酰化  肟化
收稿时间:2006-10-26
修稿时间:2006-10-262007-01-09

SYNTHESIS OF 5-NONYLSALICYALDEHYDE OXIME
Li Xiaojun,Wang Kai,Chen Wei,Feng Cheng,Li Chunying.SYNTHESIS OF 5-NONYLSALICYALDEHYDE OXIME[J].Speciality Petrochemicals,2007,24(3):57-59.
Authors:Li Xiaojun  Wang Kai  Chen Wei  Feng Cheng  Li Chunying
Affiliation:School of Chemical Engineering, Hebei University of Technology, Tianjin 300130, China
Abstract:5-Nonylsalicyaldehydeoxime was prepared from 4-nonylphenol,paraformaldehyde and hy- droxylamine 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 hydro- chloride)=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 ~(13)C NMR analysis.Comparing to the literature methods,the yield was increased by 7%.
Keywords:5-nonylsalicyaldehyde oxime  4-nonylphenol  formylation  oximation
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