摘要
以反式丙基双环己基甲酸和3,4-二氟溴苄为原料,经过还原、酯化、格氏反应和催化偶联反应最终制备了标题化合物。其中格氏偶联反应中催化剂选择Li2CuCl4,溶剂选择THF,反应时间3 h,纯化后目标产物纯度>99.7%(GC),总收率约58%,其结构经IR、1HNMR及GC-MS确证。
1,2-Difluoro- [ 2- （ trans, trans4 ＇-propylbicyclohex- yl） ethyl] benzene liquid crystal compound was synthesized from trans-4＇-propyl-（ 1, 1 ＇-bicyclohexyl ）-4-carboxylic acid and 3,4-difluorobenzyl bromide by reduction, esterification, grignard reaction and coupling reaction. The optimal condi- tions for the coupling reaction were as follows：the catalyst was Li2CuCI4 ,reaction time was 6 h,the best solvent was THF. The overall yield and purity of the target compound was about 58% and 99.7% （GC）,the structure was confirmed by IR, 1HNMR and GC-MS.
出处
《化学试剂》
CAS
CSCD
北大核心
2013年第1期62-64,共3页
Chemical Reagents
基金
北京市2011年中小企业(工业)发展专项资金资助项目(京财经一指[2011]1756号)
