两步法合成王朝酮的工艺研究  

Technology for two-step synthesis of aroma chemical dynascone

作　　者：马洪亮 李锐 吴奇林 姜兴涛 

机构地区：[1]深圳波顿香料有限公司,广东深圳518051

出　　处：《日用化学工业》2014年第11期635-637,共3页China Surfactant Detergent & Cosmetics

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。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 dynaseone. The overall yield of the two steps achieves 40. 8%. The product was characterized by IR, 1HNMR, 13 CNMR and GC - MS. Effect of dosage of the catalyst, reaction temperature and catalyst reusing on yield of 1 - acetyl - 5,5 - dimethyl - 1 - eyelohexene was investigated. Results showed that yield of 1 - aeetyl - 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.

关 键 词：王朝酮 脱氢芳樟醇 多聚磷酸 

分 类 号：TQ655[化学工程—精细化工]