[Bmim]Br-AlCl_3离子液体催化合成二-(3,4-二甲氧基苯基)乙二酮  

SYNTHESIS OF BIS-(3,4-DIMETHOXY-PHENYL) ETHANEDIONE CATALYZED BY IONIC LIQUIDBR-AlCl_3

作　　者：张文秀[1] 陈永杰[1] 李行[1] 王思林[1] 耿秀娟[1] 

机构地区：[1]沈阳化工大学应用化学学院,辽宁沈阳110142

出　　处：《精细石油化工》2012年第3期10-13,共4页Speciality Petrochemicals

摘　　要：以自制1-丁基-3-甲基咪唑溴盐-三氯化铝([Bmim]Br-AlCl3)离子液体为催化剂及反应溶剂,催化邻二甲氧基苯与草酰氯的Friedel-Crafts酰基化反应,合成二-(3,4-二甲氧基苯基)乙二酮。研究了几种不同Lew-is酸离子液体、离子液体用量、原料配比、反应温度和反应时间对酰化反应收率的影响。确定了较优的工艺条件:n([Bmim]Br-AlCl3)∶n(邻二甲氧基苯)=1∶1,n(邻二甲氧基苯)∶n(草酰氯)=1∶3,反应温度为15℃,反应时间为8h,在此条件下收率为55.76%。中间体[Bmim]Br及产物二-(3,4-二甲氧基苯基)乙二酮的结构经IR、1 H NMR确证。Abstract： Bis-（3,4-dimethoxy-phenyl）ethanedione was synthesized via Friedel-Crafts acylation reac- tion with o-dimethoxy benzene and oxalyl chloride as raw materials, bromide 1-butyl-3-methylimidazo- lium-alchlor（[Bmim]Br-A1C13） ionic liquid as catalyst and reaction solvent. Influencing factors on reaction,such as different kinds Lewis acid ionic liquid, dosage of [Bmim]Br-A1C13, ratio of raw materi- al, reaction temperature and reaction time were investigated. Experimental results show that the opti- mum conditions are n（[Bmim]Br-A1C13） ： n（o-dimethoxy benzene）=1 ： 1,n（o-dimethoxy benzene） n （oxalyl chloride） = 1 ： 3, reaction temperature was 15 ~C, reaction time was 8 h. Under the condi- tions, the yield is 55.76%. The structure of the intermediate [Bmim]Br and product bis-（3,4-dime- thoxy-phenyl）ethanedione are characterized by IR, 1H NMR.

关 键 词：离子液体 二-(3 4-二甲氧基苯基)乙二酮 Friedel-Crafts酰基化 

分 类 号：TQ426.94[化学工程]