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日用化学工业（中英文）

日用化学工业 ›› 2014, Vol. 44 ›› Issue (11): 635-637.doi: 10.13218/j.cnki.csdc.2014.11.142

• 开发与应用 • 上一篇    下一篇

两步法合成王朝酮的工艺研究

马洪亮, 李锐, 吴奇林, 姜兴涛   

  1. 深圳波顿香料有限公司,广东 深圳 518051
  • 收稿日期:2014-05-30 出版日期:2014-11-22 发布日期:2019-04-08
  • 作者简介:马洪亮(1982-),男,河北廊坊人,工程师,电话:18938906975,E-mail:mahongliang20000@163.com。

Technology for two-step synthesis of aroma chemical dynascone

MA Hong-liang, LI Rui, WU Qi-lin, JIANG Xing-tao   

  1. Boton Flavors & Fragrances Co.,Ltd.,Shenzhen,Guangdong 518051,China
  • Received:2014-05-30 Online:2014-11-22 Published:2019-04-08

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摘要： 以脱氢芳樟醇为原料,先在多聚磷酸(PPA)的催化下进行重排,同时发生环化后得到1-乙酰基-5,5-二甲基-1-环己烯,然后再进行烷基化反应生成目标产物王朝酮,两步反应的总产率达40.8%。产物用IR,1HNMR,13CNMR和GC-MS等进行了表征。探讨了反应温度、催化剂用量及催化剂重复使用次数对中间体1-乙酰基-5,5-二甲基-1-环己烯产率的影响,结果表明:反应温度为80 ℃,脱氢芳樟醇与多聚磷酸的质量比为1:2条件下中间体产率较高,可达到97.0%,催化剂多聚磷酸可重复使用2~3次。

关键词: 王朝酮, 脱氢芳樟醇, 多聚磷酸

Abstract: Firstly 1-acetyl-5,5-dimethyl-1-cyclohexene was obtained via rearrangement cyclization reaction with dehydrolinalool as starting material and poly-phosphoric acid (PPA) as catalyst,and then via the alkylation reaction to synthesize the targeted product dynascone.The overall yield of the two steps achieves 40.8%.The product was characterized by IR,1HNMR,13CNMR and GC-MS.Effect of dosage of the catalyst,reaction temperature and catalyst reusing on yield of 1-acetyl-5,5-dimethyl-1-cyclohexene was investigated.Results showed that yield of 1-acetyl-5,5-dimethyl-1-cyclohexene achieves 97.0% based on 80 ℃ of reaction temperature and mass ratio of dehydrolinalool to PPA 1:2.The catalyst PPA can be reused for 2~3 times.

Key words: dynascone, dehydrolinalool, poly-phosphoric acid

中图分类号: 

  • TQ655