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含氟苯环环己基噁烷类液晶化合物的合成新法

A new method of synthesis of fluorinated phenyl cyclohexyl dioxane liquid crystal compounds

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【作者】 侯修泽巨妮娟段迎春高仁孝

【Author】 HOU Xiu-ze;JU Ni-juan;DUAN Ying-chun;GAO Ren-xiao;Xi’an Ruilian Modern Electronic Materials Co.,Ltd.;

【机构】 西安瑞联近代电子材料有限责任公司

【摘要】 以4-烷基环己酮和丙二腈为原料,经Knoevenagel反应获得2-烷基环己基亚甲基丙二腈,通过Na BH4选择性加氢得到2-烷基环己基丙二腈,经水解、还原得到2-烷基环己基丙二醇,再与3,4,5-三氟苯甲醛发生分子间脱水和环,合成了一系列不同烷基的2-(3,4,5-三氟苯基)-5-(4-烷基环己基)-1,3-噁烷。GC质量含量> 99. 5%,收率达10%~14%,较专利文献[1]收率(1%~3%)有显著提高。通过质谱、核磁、红外光谱以及差示扫描量热法(DSC)对目标产物的结构和相变行为进行了测试。

【Abstract】 A series of fluorinated phenyl cyclohexyl dioxane compounds are synthesized by a new process using 4-alkyl cyclohexanone and malononitrile as starting material through Knoevenagel,selective hydrogenation,hydrolyzation,reduction,then carried out 2-alkyl cyclohexyl 1,3-propanediol. It reacted with 3,4,5-trifluobenzo formaldehyde by intramolecular dehydration,and came into being 5-(4-alkylcyclohexyl)-2-(3,4,5-trifluorophenyl)-1,3-dioxane. The yields(10% ~ 14%) are much higher than reported in the literatures(1% ~ 3%). The GC purity of the products are higher than 99.5%. All these compounds are identified by GC-MS,1 HNMR,FTIR,and their phase transition behaviors are studied by DSC.

【关键词】 液晶合成噁烷含氟
【Key words】 liquid crystalsynthesisdioxanefluorinated
  • 【文献出处】 应用化工 ,Applied Chemical Industry , 编辑部邮箱 ,2014年S2期
  • 【分类号】O753.2
  • 【下载频次】50
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