期刊文献+

N-羟基邻苯二甲酰亚胺/Co(acac)_2催化的α-紫罗兰酮的氧化反应 被引量:1

Aerobic Oxidation of α-Ionone Catalyzed by N-Hydroxyphthalimide Combined with Co(acac)_2
下载PDF
导出
摘要 以分子氧(O2)为氧化剂,在无溶剂条件下,研究了N-羟基邻苯二甲酰亚胺/乙酰丙酮亚钴(Ⅱ)体系对α-紫罗兰酮的催化氧化反应,分析了氧化产物,主要得到α-紫罗兰酮的烯丙位氧化产物5-氧代-α-紫罗兰酮,同时生成少量环氧α-紫罗兰酮及重排产物4-氧代-β-紫罗兰酮和环氧β-紫罗兰酮,提出了可能的反应机理,化合物的结构经IR、1H NMR、MS和EA等测试技术得以表征;为了提高5-氧代-α-紫罗兰酮的选择性和催化氧化反应的转化率,优化了催化氧化反应的工艺条件:当反应温度为70℃,氧气压力为1.0 MPa,N-羟基邻苯二甲酰亚胺和乙酰丙酮亚钴(Ⅱ)用量分别为α-紫罗兰酮的25%和1.0%,反应10 h,5-氧代-α-紫罗兰酮的产率达53.4%,反应转化率达95.0%以上,平行实验表明,实验重复性良好。 A practical catalytic method to oxidize α-ionone with molecular oxygen under normal pressure and temperature in the presence of catalyst N-hydroxyphthalimide(NHPI) combined with Co(acac)2 was developed,and the probable catalytic mechanism was proposed.Influences of the reaction conditions on the conversion of α-ionone and the selectivity of the major product(5-oxo-α-ionone) were investigated,the optimal technical parameters for 5-oxo-α-ionone were optimized.The results show that the primary products were 5-oxo-α-ionone,epoxy-α-ionone,as well as rearrangement products 4-oxo-β-ionone and epoxy-β-ionone,which were characterized by infrared spectroscopy,1H nuclear magnetic resonance spectroscopy,mass spectrometry and elemental analysis.The yield of 5-oxo-α-ionone and the conversion of α-ionone were 53.4% and 95.0%,respectively,under the conditions of 25% NHPI,1.0% Co(acac)2(in molar ratio),O2 pressure of 1.0 MPa,the reaction temperature at 70 ℃,and reaction time of 10 h,the procedure shows a good reprodu-cibility in the parallel experiments.
出处 《应用化学》 CAS CSCD 北大核心 2009年第11期1305-1309,共5页 Chinese Journal of Applied Chemistry
关键词 N-羟基邻苯二甲酰亚胺 催化氧化 α-紫罗兰酮 氧代-α-紫罗兰酮 N-hydroxyphthalimide, catalytic oxidation, α-ionone, oxo-α-ionone
  • 相关文献

参考文献1

  • 1彭黔荣,杨敏,谢如刚,宋光富,刘钟祥,王东山,蔡元青.一步法合成酮代α-紫罗兰酮,酮代β-紫罗兰酮及其醚、酯类衍生物[P]中国专利:CN1817842.

同被引文献7

引证文献1

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部