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3,5-二烷基-4-羟基苯甲腈的一步法合成
ONE-POT SYNTHESES OF 3,5-DIALKYL-4-HYDROXYBENZONITRILES
【摘要】 实验以3,5-二烷基-4-羟基苯甲醛(烷基为甲基、异丙基和叔丁基)和NH2OH.HCl为原料,在HCOOH、HOAc和DMF 3种溶剂中一步法合成相应的苯甲腈。考察了原料配比、反应温度等对产物收率的影响。结果表明,合成3,5-二甲基-4-羟基苯甲腈的最优条件为:醛用量0.16 mol,n(醛)∶n(羟胺)=1∶1.2,DMF用量80 mL,温度105℃,反应6 h,收率93.5%;合成3,5-二异丙基-4-羟基苯甲腈的较优条件为:n(醛)∶n(羟胺)=1∶1.2,DMF用量100 mL,温度105~110℃,反应6 h,收率88.0%;合成3,5-二叔丁基-4-羟基苯甲腈的较优条件为:n(醛)∶n(羟胺)=1∶1.2,HOAc用量100 mL,温度105~110℃,反应6 h,收率99%以上。
【Abstract】 The one-pot syntheses of 3,5-dialkyl-4-hydroxybenzonitriles(alkyl= methyl,isopropyl and tert-butyl) from the corresponding benzaldehydes and NH2OH·HCl in HCOOH,HOAc,and DMF,respectively,were studied.The highest yields of 3,5-dimethyl-4-hydroxybenzonitrile,3,5-di-isopropyl-4-hydroxybenzonitrile and 3,5-di-tert-butyl-4-hydroxybenzonitrile were 93.5%,88.0% and 99%,respectively,under optimal conditions.
- 【文献出处】 精细石油化工 ,Speciality Petrochemicals , 编辑部邮箱 ,2010年03期
- 【分类号】TQ246.7
- 【下载频次】247