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。
The one-pot syntheses of 3,5-dialkyl-4-hydroxybenzonitriles （alkyl= methyl, isopropyl and tert-butyl） from the corresponding benzaldehydes and NH2 OH - HCl in HCOOH, HOAc, and DMF, respectively, were pyl-4-hydroxybenz 99%, respectively studied. The highest yields of 3,5-dimethyl-4-hydroxybenzonitrile, 3,5-di-isopro- onitrile and 3, 5-di-tert-butyl- 4-hydroxybenzonitrile were 93.5%, 88.0% and , under optimal conditions.
出处
《精细石油化工》
CAS
CSCD
北大核心
2010年第3期48-51,共4页
Speciality Petrochemicals
