有色金属科学与工程
有色金屬科學與工程
유색금속과학여공정
JIANGXI NONFERROUS METALS
2014年
5期
97-100
,共4页
对特辛基苯酚%2-羟基-5-特辛基苯乙酮肟%Fries重排%肟化
對特辛基苯酚%2-羥基-5-特辛基苯乙酮肟%Fries重排%肟化
대특신기분분%2-간기-5-특신기분을동우%Fries중배%우화
p-(tert-octyl)phenol%2-hydroxy-5-octyl phenyl ethyl ketoxime%Fries rearrangement%oximation
以四氯乙烯为溶剂，对特辛基苯酚、乙酰氯、无水AlCl3和盐酸羟胺为主要原料，采用分步合成法合成了2-羟基-5-特辛基苯乙酮肟.考察了无水AlCl3用量、乙酰氯的用量、Fries重排温度、肟化反应盐酸羟胺用量以及缚酸剂无水碳酸钠用量对产物产率的影响，实验结果表明，当n（AlCl3）∶n（乙酰氯）∶n（对特辛基苯酚）=1.5∶2∶1，Fries重排温度为120℃，n（Na2CO3）∶n（盐酸羟胺）∶n（对特辛基苯酚）=0.5∶1∶1.产物收率64.9%.对合成产物利用核磁共振进行了结构表征.
以四氯乙烯為溶劑，對特辛基苯酚、乙酰氯、無水AlCl3和鹽痠羥胺為主要原料，採用分步閤成法閤成瞭2-羥基-5-特辛基苯乙酮肟.攷察瞭無水AlCl3用量、乙酰氯的用量、Fries重排溫度、肟化反應鹽痠羥胺用量以及縳痠劑無水碳痠鈉用量對產物產率的影響，實驗結果錶明，噹n（AlCl3）∶n（乙酰氯）∶n（對特辛基苯酚）=1.5∶2∶1，Fries重排溫度為120℃，n（Na2CO3）∶n（鹽痠羥胺）∶n（對特辛基苯酚）=0.5∶1∶1.產物收率64.9%.對閤成產物利用覈磁共振進行瞭結構錶徵.
이사록을희위용제，대특신기분분、을선록、무수AlCl3화염산간알위주요원료，채용분보합성법합성료2-간기-5-특신기분을동우.고찰료무수AlCl3용량、을선록적용량、Fries중배온도、우화반응염산간알용량이급박산제무수탄산납용량대산물산솔적영향，실험결과표명，당n（AlCl3）∶n（을선록）∶n（대특신기분분）=1.5∶2∶1，Fries중배온도위120℃，n（Na2CO3）∶n（염산간알）∶n（대특신기분분）=0.5∶1∶1.산물수솔64.9%.대합성산물이용핵자공진진행료결구표정.
2-hydroxy-5-octyl phenyl ethyl ketoxime is prepared by three-step method using tetrachloroethylene as solvent, p-(tert-octyl)phenol, acetyl chloride, anhydrous aluminum chloride and hydroxylamine hydrochloride as raw materials. The effects of anhydrous aluminum chloride dosage, acetyl chloride dosage, Fries rearranging temperature, dosages of hydroxylamine hydrochloride and acid-binding agent anhydrous sodium carbonate in oximation reaction on the yield of 2-hydroxy-5-octyl phenyl ethyl ketoxime are investigated. The results show that the reaction rate of 2-hydroxy-5-octyl phenyl ethyl ketoxime production yield reaches 64.9 % under optimum reaction conditions: the mole ratio of anhydrous aluminum chloride, acetyl chloride and p-(tert-octyl) phenol is 1.5:2:1. Fries rearranging temperature is 120 ℃ and the mole ratio of anhydrous sodium carbonate, acetyl chloride and p-(tert-octyl)phenol is 0.5:1:1. The molecular structure of the product is characterized with nuclear magnetism resonance spectrum.
