过氧化氢环氧化β-蒎烯合成2,10-环氧蒎烷
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TQ651

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国家科技支撑计划项目(2011BAD23B01);北京市属高等学校人才强教计划资助项目(PHR20090504);北京工商大学研究生科研学术创新基金项目


Synthesis of 2,10-Epoxypinane by Epoxidation of β-pinene with Hydrogen peroxide
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    摘要:

    以β-蒎烯为原料,乙腈-水为溶剂,酮为催化剂,过氧化氢为氧化剂,进行环氧化反应合成2,10-环氧蒎烷。考察了酮催化剂、溶剂、过氧化氢与β-蒎烯摩尔比、pH值、反应温度和时间对2,10-环氧蒎烷产率的影响。实验结果表明,丙酮为较佳的催化剂, n (过氧化氢): n (β-蒎烯)=5:1,体系pH=10.0,反应温度30℃,反应时间8h时,2,10-环氧蒎烷的收率可达79.6%,纯度为94.6% 。用气相色谱、气-质联机、红外光谱以及1H核磁共振谱图对2,10-环氧蒎烷的纯度和结构进行了表征。

    Abstract:

    2,10-Epoxypinane was synthesized by the epoxidation of β-pinene using acetonitrile-water as solvent, ketone as catalyst, hydrogen peroxide as oxidant. The effect of ketone, solvent, mole ratio of hydrogen peroxide to β-pinene , pH, reaction temperature and time on the yield of 2,10-epoxypinane was investigated. The results show that the yield of 2,10-epoxypinane could reach 79.6% and its content was 94.6% under the following reaction conditions: the proper catalyst was acetone, the mole ratio of hydrogen peroxide to β-pinene was 5:1, pH was 10.0 , reaction temperature was 30℃,and the reaction time was 8h. The product was characterized by data of GC, GC-MS spectrum, infrared spectrum and 1H NMR spectrum.

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贺香文,郑福平.过氧化氢环氧化β-蒎烯合成2,10-环氧蒎烷[J].精细化工,2011,28(10):

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  • 收稿日期:2011-07-06
  • 最后修改日期:2011-07-29
  • 录用日期:2011-08-22
  • 在线发布日期: 2011-09-29
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