摘要
以3-氟溴苯、对溴苯腈、丙基环己基甲基氯等为原料,经过格氏反应、Suzuki反应、Witting反应、氢化反应等7步反应最终合成出化合物2,6-二氟-4-{3-氟_4’-[1-甲基-2-(4-丙基环己基)-乙基]联苯}苯基二氟甲氧基-3,4,5-三氟苯[化合物(Ⅶ)],其中格氏试剂与对溴苯腈的反应中溶剂选择二甲苯;锂化反应制备硼酸中,锂化反应时间选择2h;纯化后目标产物气相色谱纯度为99.7%(熔点82.97-85.04℃),总收率约为30%,其结构经IR、HNMR及GC—MS确证。该化合物添加到液晶的基础配方中,能提高配方的双折射率(△凡),降低其阈值电压(Vth)。
Using 1-bromo-3-fluorobenzene,4-bromobenzonitrile,1-(trans-4-propylcyclohexyl)-1-chloro-methane as starting materials,2,6-difluoro-4-t 3-fluoro-4'-[1-methyl-2-(4-propylcyclohexyl)-ethyl]-biphenyl/phenyl difluoromethoxy-3,4,5-trifluorobenzene was synthesized by a method consisting of seven steps,including Grignard reaction,Suzuki reaction,Witting reaction,hydrogenation reaction,etc.The reaction solvent of Grignard reagent and 4-bromobenzonitrile was xylene,and the optimum reaction time of lithiation reaction was 2 h.The overall yield was about 30%and the purity reached 99.7%(GC)(rap:82.97-85.04℃).The addition of the compound into the basic formula of liquid crystal can improve the birefringence(An)and reduce the threshold voltage(Vth).
作者
杭德余
班全志
姜天孟
田会强
储士红
HANG De-yu;BAN Quan-zhi;JIANG Tian-meng;TIAN Hui-qiang;CHU Shi-hong(Beijing Key Laboratory of Liquid Crystal Materials Analysis and Application Technology,Beijing Bayi Space Liquid Crystal Material Technology Company,Beijing 102205,China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第11期1204-1207,1228,共5页
Fine Chemicals
