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一步法合成5-叔丁基-1,2,3-三甲基苯

Synthesis of 5-tert-butyl-1, 2,3-trimethylbenzene by One Step

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【作者】 黄荣荣马江权李桂云姚致远

【Author】 HUANG Rong-rong, MA Jiang-quan, LI Gui-yun, YAO Zhi-yuan (Key Laboratory of Fine Chemical Engineering,Jiangsu Institute of Petrochemical Technology, Changzhou 213016,China)

【机构】 江苏石油化工学院精细化工重点实验室! 江苏 常州 213016

【摘要】 介绍了以C9重芳烃中的连三甲苯和氯代叔丁烷为起始原料在自制的非均相催化剂W100的作用下,一步合成生产三甲苯麝香的中间体5-叔丁基-1,2,3-三甲基苯的简便方法。经探索性试验和正交试验得出如下优化条件:连三甲苯与氯代叔丁烷摩尔比为1:1,催化剂W100与连三甲苯质量比为0.02:1,反应温度3~5℃,反应时间7h,在此条件下5-叔丁基-1,2,3-三甲基苯的收率达到78%。通过色质联用GC/MS对产品进行了定性和定量分析,产品的比重=0.8791 ,折光率=1.5030,熔点为30.2~30.6℃。本法工艺简单,原料价格便宜,产品收率高,有较好的工业应用前景。

【Abstract】 : The paper introduced the process of preparing 5-tert- butyl-1, 2,3-trimethylbenzene which was the intermediate to produce musk tibetene by one step in the presence of heterogeneous catalyst W100 (home-made), and using 1,2,3-trimethylbenzene from C9 heavy aromatics and 2-chloro-iso-butane as raw materials. Based on trial test and orthogonal test the suitable conditions were established. The optimum reaction conditions were as follows 1,2,3-trimethylbenzene/2-chloro-iso-butane molar ratio 1:1, W100 catalyst/1,2,3-trimethylbenzene mass ratio 0.02:1, reaction temperature 3~5℃ , reaction time 5h. The yield of product was about 78%. The composition and structure of 5-tert-butyl-1, 2,3- trimethyl-benzene were further analyzed through GC/MS.Some physicochemical property of product were measured: specific density = 0.8791, refractive index =1.5030, melting point equals to 30.2~30.6℃,the product quality was up to the literature standard. This process had many advantages such as simpler procedure, shorter reaction period, cheaper raw material, higher yield, etc. So the route had good prospect for industrialization.

【基金】 金陵石化公司资助项目!(97032L)
  • 【文献出处】 高校化学工程学报 ,Journal of Chemical Engineering of Chinese Universities , 编辑部邮箱 ,2000年06期
  • 【分类号】TQ24
  • 【被引频次】7
  • 【下载频次】144
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