间三氟甲基苯乙烯的合成  

SYNTHESIS OF m-TRIFLUOROMETHYL STYRENE

作　　者：廖云峰[1] 陈红飙[1] 彭智勇[1] 刘进兵[1] 谭丹[1] 林原斌[1] 

机构地区：[1]湘潭大学化学学院,湖南湘潭411105

出　　处：《精细石油化工》2005年第1期40-43,共4页Speciality Petrochemicals

基　　金：湖南省教育厅资助项目(03C461)

摘　　要：以间三氟甲基苯胺为起始原料,经重氮化、甲醛肟甲酰化、缩合、脱羧四步反应,合成了高纯度的间三氟甲基苯乙烯,总收率为17.6%,并用FT-IR,1HNMR进行了表征。结果表明,最佳反应条件为:在缩合反应中,n(间三氟甲基苯甲醛):n(丙二酸):n(吡啶):n(无水乙醇)=1:1.11:0.17:3.98,回流时间6h;在脱羧反应中,反应温度220℃,反应时间2h。High purity m-trifluoromethyl styrene was synthesized from m-trifluoromethyl- aniline with the overall yield of 17. 6% through four steps, including diazotization, acylation of formaldoxime, condensation and decarboxylation. The structure of the products was characterized by FT-IR and 1 H NMR. The results showed that the optimal synthetic conditions were as follows: n(m-trifluorometh-ylbenzaldehyde) : n(malonic acid) : n(pyridine) : n(anhydrous ethanol) = l : 1. 11 : 0. 17 : 3. 98, the refluxing time is 6 h for the reaction of condensation; and the reaction temperature is 220 ℃, the reaction time is 2 h for the reaction of decarboxylation.

关 键 词：间三氟甲基苯胺 苯乙烯 合成 起始原料 总收率 并用 高纯度 最佳反应条件 苯甲醛 甲酰化 

分 类 号：TE624.99[石油与天然气工程—油气加工工程] TQ242.1[化学工程—有机化工]