3-甲基吲哚的合成工艺研究  

Research on the synthesis of 3-methylindole

作　　者：宋岩[1] 田振生[2] 张吉波[1] 

机构地区：[1]吉林化工学院化工与材料学院,吉林吉林132022 [2]中国石油吉林石化公司研究院,吉林吉林132021

出　　处：《化工科技》2011年第6期31-33,共3页Science & Technology in Chemical Industry

基　　金：中国石油天然气集团公司应用基础研究项目(06A50201)

摘　　要：3-甲基吲哚是一种重要的精细化工原料,可用于日用香精及食用香精的调配,作为定香剂使用。作者以丙醛和苯肼为原料,经缩合反应脱水生成丙醛苯腙,丙醛苯腙在高温下发生环化反应,最终得到产品3-甲基吲哚,分别考察了缩合过程中反应物投料比、环化反应过程中投料比及催化剂用量等条件对反应的影响。实验结果表明,当缩合反应n(丙醛):n(苯肼)=1.08:1,m(环己烷):m(苯肼)=0.8:1,丙醛苯腙的收率可达到92.67%;在环化反应过程中溶剂m(二甲苯):m(丙醛苯腙)=1.4:1.0,m(催化剂):m(丙醛苯腙)=7.5%时,总收率可以达到74.17%,产品熔点为96.1～97.2℃。3-Methylindole is apromising material in fine chemicals,it may use in the daily essence,flavoring agent,and perfume fixative.In this article,we used the propionic aldehyde and hydrazinobenzene as raw materials.Via condensation dehydration reaction We synthezed propylaldehyde phenylhydrazone,which underwent cyclization reaction at the high temperature,obtain successfully 3-methylindole.In addition,we investigated the effect of the ratio of raw materials in condensation reaction,the ratio of raw materials and catalyst level in cyclization reaction.It has been proved that in condensation reaction the mole ratio of propionic aldehyde to hydrazinobenzene was 1.08∶1,the ratio of the quality for cyclohexane to hydrazinobenzene was 0.8∶1.0,the yield of propylaldehyde phenylhydrazone was 92.67%;in cyclization reaction the the ratio of the quality for dimethylbenzene to propionic aldehyde was 1.4∶1,catalyst level was 7.5% of propylaldehyde phenylhydrazone.Finally,the total yield may achieve 74.17%,3-methylindole was obtained with melting point of 96.1~97.2 ℃.

关 键 词：3-甲基吲哚 定香剂 缩合反应 环化反应 

分 类 号：TQ251.34[化学工程—有机化工]