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对羟基苯甲腈合成方法的改进
Study on one-pot preparation of 4-hydroxybenzonitrile
【摘要】 研究了对羟基苯甲醛与盐酸羟胺在N ,N- 二甲基甲酰胺中合成对羟基苯甲腈的反应 ,在n盐酸羟胺 :n对羟基苯甲醛 =1 2∶1 0 ,反应温度为 110~ 12 0℃时反应 5h ,溶剂N ,N- 二甲基甲酰胺回收后 ,对羟基苯甲腈经减压蒸馏和重结晶提纯 ,收率可达 86 . 0 % ,含量 99 .9% ;产物用元素分析、IR、1HNMR进行了确证。
【Abstract】 One-pot preparation of 4-hydroxybenzonitrile by the r eaction of 4-hydroxybenzaldehyde and hydroxylamine hydrochloride in N,N-di methyl formamide(DMF) was studied.The optimum process conditions were determined :n (hydroxylamine hydrochloride)∶n (4-hydroxybenzaldehyde)=1 .2∶1.0,reaction time 5h and reaction temperature 110~120℃.4-Hydroxybenzoni trile was purified by distillation in vacuum and recrystallization after DMF was recovered.The yield of 4-hydroxybenzonitrile was 86.0% ,and the assay was 99 .9%.The product was confirmed by elemental analysis,IR and 1HNMR.
【Key words】 hydroxybenzonitrile; 4-hydroxybenzaldehyde; N,N -dimethylformamide; preparation;
- 【文献出处】 化学试剂 ,Chemical Reagents , 编辑部邮箱 ,2005年03期
- 【分类号】TQ246
- 【被引频次】10
- 【下载频次】701