摘要
以2,3-二氟苯乙醚和乙酰氯为起始原料,经傅克反应合成了质量分数99%以上的液晶中间体4-乙氧基-2,3-二氟苯乙酮,对目标化合物进行了1HNMR、IR和GC-MS表征。以二氯甲烷为反应溶剂,当n(2,3-二氟苯乙醚)∶n(三氯化铝)∶n(乙酰氯)=1∶1.14∶1.3,反应温度为-10～-5℃,反应时间为1 h时,反应效果最佳,产物质量分数为89.2%,2,3-二氟苯乙醚质量分数为4.83%,副产物4-乙酰基-2,3-二氟苯酚醋酸酯质量分数为0.12%,产物异构体未检出。根据实验结果对傅克反应副产物产生的原因进行了推测。
The liquid crystal intermediate 4-ethoxy-2,3-difluoroacetophenone of a purity of more than 99% was synthesized via Friedel-Crafts reaction with 2,3-difluoroethoxybenzene and acetyl chloride as starting materials. The target compound was characterized by means of 1HNMR, IR and GC - MS. When dichloromethane was used as reaction solvent, the molar ratio of 2,3-difluoroethoxybenzene/aluminium chloride/acetyl chloride was 1：1.14：1.3,the reaction temperature was -10 - -5℃ and the reaction time was 1 h, the reaction results was best, with the mass ratio of the main product being 89.2%, the mass ratio of 2,3-difluoroethoxybenzene being 4.83%, the mass ratio of 4-acetyl-2,3-difluorophenyl acetate being 0. 12% and the content of the isomers of the product being not detected. The generation reason of the by-products during Friedel-Crafts reaction was proposed according to the results of the experiments.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第2期232-234,共3页
Fine Chemicals
