谢光勇,罗德荣,张 莉,陈 雄,曾 艺,黄业迎.直接碘化反应高效合成碘代芳烃[J].中南民族大学学报自然科学版,2018,(2):1-5
直接碘化反应高效合成碘代芳烃
Efficient Synthesis of Iodine-substituted Aromatics by Direct Iodination
  
DOI:10.12130/znmdzk.20180201
中文关键词: 碘代芳烃  3-叔丁基水杨醛  3-叔丁基-5-碘水杨醛  碘化反应  合成
英文关键词: iodine-substituted aromatics  3-tert-butylsalicylaldehyde  3-tert-butyl-5-iodosalicylaldehyde  iodination  synthesis
基金项目:国家自然科学基金资助项目(21172269)
作者单位
谢光勇,罗德荣,张 莉,陈 雄,曾 艺,黄业迎 中南民族大学 化学与材料科学学院催化材料科学国家民委-教育部共建重点实验室武汉 430074 
摘要点击次数: 651
全文下载次数: 308
中文摘要:
      以3-叔丁基水杨醛为原料,通过3种不同的碘化方法分别合成了3-叔丁基-5-碘水杨醛,在温和条件下,以水-乙醇为溶剂、KI为碘化试剂、H2O2为氧化剂有效合成了3-叔丁基-5-碘水杨醛.结果表明: 在水/乙醇体积比为3︰1,H2SO4的质量浓度为62.5 mg·mL-1,反应物/KI/氧化剂摩尔比为1︰1︰2,反应温度为70 ℃,反应时间为6 h时,碘取代反应条件最佳.此时,3-叔丁基-5碘水杨醛摩尔收率高达88.1%, 2,6-二氟苯胺和2,6-二异丙基苯胺在该条件下成功进行了碘化反应,产物摩尔收率分别可达87.3%和85.6%.
英文摘要:
      3-tert-butyl-5-iodosalicylaldehyde was synthesized through three different iodination methods using 3-tert-butylsalicylaldehyde as starting material. Efficient synthesis of 3-tert-butyl-5-iodosalicylaldehyde under mild conditions was achieved by using water-ethanol as solvent, potassium iodide as iodination reagent and hydrogen peroxide as oxidant. The optimum reaction conditions were found as follows: 3︰1, volume ratio of water to ethanol; 62.5 mg·mL-1, mass concentration of sulfuric acid; 1︰1︰2, molar ratio of reactant/potassium iodide/oxidant; 70 ℃, reaction temperature; 6 h, reaction time. Under these conditions, the yield of 3-tert-butyl-5-iodosalicylaldehyde could reach 88.1%. Furthermore, iodination of 2,6-difluoroaniline and 2,6-diisopropylaniline could also be realized through this method, with 87.3% and 85.6% of yields respectively.
查看全文   查看/发表评论  下载PDF阅读器
关闭