萃取剂2-羟基-5-壬基苯乙酮肟的合成  

The synthesis of extractant 2-hydroxy-5-nonylacetophenone oxime

作　　者：李效军[1] 冯成[1] 李春英[1] 陈炜[1] 

机构地区：[1]河北工业大学化工学院,天津300130

出　　处：《天津化工》2007年第1期21-22,28,共3页Tianjin Chemical Industry

摘　　要：本文以4-壬基酚、乙酰氯、无水AlCl3和盐酸羟胺为主要原料合成了2-羟基-5-壬基苯乙酮肟(HNAO)。合成2-羟基-5-壬基苯乙酮(HNA)时,采用了一步法,以四氯乙烯为溶剂,n(4-壬基酚)∶n(乙酰氯)∶n(AlCl3)=1∶2∶1.2,加毕AlCl3后补加4-壬基酚物质量0.2倍的乙酰氯,回流温度下(120℃)反应6h。HNA收率为98.1%,纯度为79.5%。合成HNAO时,以蒸馏的HNA为原料,以甲苯为溶剂,导辛酸钠为相转移催化剂,n(HNA)∶n(盐酸羟安)∶n(碳酸钠)=1∶1.3∶0.85,75℃下反应4.5h。HNAO收率为97.9%,纯度为88.6%。FT-IR分析结果表明所得中间体及产物与HNA和HNAO特征相符。2-Hydroxy-5-nonylacetophenone oxime was synthesized from 4-nonylphenol, acetyl chloride, aluminum chloride and hydroxylamine hydrochloride in this paper. While preparing 2-hydroxy-5-nonylacetophenone one-pot method was employed, thus tetrachloro ethylene was selected as solvent, n（4-nonylphenol）：n（acetyl chloride）：n （AlCl3） was 1：2：1.2, the molecular ratio of additional acetyl chloride to 4-nonylphenol was 0.2：1 on completion of addition of aluminum chloride, the reaction was carried out under reflux （120℃） for 6h. The yield of the 2-Hydroxy- 5-nonylacetophenone based on 4-nonylphenol was 98.1% and the purity of the 2-hydroxy-5-nonylacetophenone was 79.5%. While preparing 2-hydroxy-5-nonyl-aeetophenone oxime the distilled 2-hydroxy-5-nonylacetophenone was used and toluene was used as solvent, sodium ethylhexanate was used as PTC, n（HNA）：n（hydroxylamine）：n（Na2CO3） =1：1.3：0.85, the reaction was carried out under 75~C for 4.5h. The yield of the 2-hydroxy-5-nonylacetophenone oxime based on 2-hydroxy-5-nonylacetophenone was 97.9% with a purity of 88.6%. The structures of the intermediate and final product were characterized by FT-IR.

关 键 词：2-羟基-5-壬基苯乙酮肟 2-羟基-5-壬基苯乙酮 FRIES重排 肟化 

分 类 号：TQ244.2[化学工程—有机化工]