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林产化学与工业 ›› 2021, Vol. 41 ›› Issue (4): 23-28.doi: 10.3969/j.issn.0253-2417.2021.04.004

• 重点研发专栏 • 上一篇    下一篇

甲基三氧化铼催化合成罗汉柏木烷酮

张胜1(), 朱凯1,2,*()   

  1. 1. 南京林业大学 化学工程学院, 江苏 南京 210037
    2. 南京林业大学 江苏省林业资源高效加工利用协同创新中心, 江苏 南京 210037
  • 收稿日期:2020-11-30 出版日期:2021-08-28 发布日期:2021-08-31
  • 通讯作者: 朱凯 E-mail:1071929101@qq.com;zhukai53@163.com
  • 作者简介:朱凯, 教授, 硕士生导师, 研究方向为香精香料; E-mail: zhukai53@163.com
    张胜(1995-), 男, 贵州遵义人, 硕士生, 从事香精香料方面研究; E-mail: 1071929101@qq.com
  • 基金资助:
    国家重点研发计划资助项目(2018YFD0600405);江苏高校优势学科建设工程项目

Synthesis of Thujopsanone Catalyzed by Methyltrioxorhenium

Sheng ZHANG1(), Kai ZHU1,2,*()   

  1. 1. College of Chemical Engineering, Nanjing Forestry University, Nanjing 210037, China
    2. Jiangsu Co-Innovation Center of Efficient Processing and Utilization of Forest Resources, Nanjing Forestry University, Nanjing 210037, China
  • Received:2020-11-30 Online:2021-08-28 Published:2021-08-31
  • Contact: Kai ZHU E-mail:1071929101@qq.com;zhukai53@163.com

摘要:

以罗汉柏木烯为原料,二氯甲烷为溶剂,甲基三氧化铼(MTO)为催化剂,H2O2为氧化剂,3-甲基吡唑为碱性配体,进行氧化反应合成罗汉柏木烷酮。考察了反应条件对氧化反应的影响,得到最佳工艺条件为:反应温度30℃,n(H2O2):n(罗汉柏木烯)=2:1,反应时间3 h,催化剂用量为0.3%(以罗汉柏木烯质量计,下同),3-甲基吡唑用量为10%。在最佳工艺条件下,产物得率为72.1%,罗汉柏木烯转化率为97.3%。采用FT-IR和GC-MS分析方法对产物进行表征,确定产物为罗汉柏木烷酮。

关键词: 罗汉柏木烷酮, 甲基三氧化铼, 氧化, 罗汉柏木烯, 3-甲基吡唑

Abstract:

Thujopsanone was synthesized by oxidation reaction with thujopsene as raw material, dichloromethane as solvent, methyltrioxorhenium(MTO) as catalyst, 30% H2O2 as oxidant, and 3-methylpyrazole as co-catalyst. The effects of reaction conditions on the oxidation were studied. The optimized reaction were obtained as follows: the reaction temperature 30℃, the molar ratio of raw materals(n(H2O2): n(thujopsene)) 1:1, the reaction time 3 h, the catalyst amounts 0.3%(based on the weight of thujopsene, similarly hereinafter), the dosage of 3-methylpyrazole is 10%. Under these conditions, the yield of thujopsanone was 72.1%, and the conversion rate of thujopsene was 97.3%. The structure of the products was identified by GC-MS and FT-IR, and it was confirmed as wasthujopsanone.

Key words: thujopsanone, MTO, oxidation, thujopsene, 3-methylpyrazole

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