FeSIL催化合成2-氨基-3,5-二溴苯甲醛  

Synthesis of 2-Amino-3, 5-Dibromobenzaldehyde Catalyzed by SBA-15 Supported Ionic Liquid FeSIL

作　　者：张宝华[1] 史兰香[1] 张之奎 ZHANG Bao-hua;SHI Lan-xiang;ZHANG Zhi-kui(School of Chemical Engineering,Shijiazhuang University,Shijiazhuang,Hebei 050035,China;Shijiazhuang Penghai Pharmacutical Co.,Ltd.,Shijiazhuang,Hebei 050600,China)

机构地区：[1]石家庄学院化工学院,河北石家庄050035 [2]石家庄鹏海制药有股份限公司,河北石家庄050600

出　　处：《石家庄学院学报》2020年第3期88-92,共5页Journal of Shijiazhuang University

基　　金：河北省科技支撑项目(19222609D);河北省科技小巨人(培育)项目(18C1303111026)。

摘　　要：以2-氨基苯甲醛和NH4Br/H2O2为原料,在SBA-15支载的1-甲基-3-(丙基三氧基硅烷)咪唑-FeBr4离子液体(FeSIL)催化作用下,经溴化反应制备了2-氨基-3,5-二溴苯甲醛.对离子液体催化剂进行了制备和筛选.考察了溴盐种类、底物投料比、催化剂用量、H2O2浓度、反应温度和反应时间对产物收率的影响.当反应温度为40℃,反应时间为3 h,n(2-氨基苯甲醛):n(NH4Br):n(H2O2):n(FeSIL)=1:3:1.1:0.03,H2O2浓度为15%时,2-氨基-3,5-二溴苯甲醛的收率达98.5%,含量99.7%.负载催化剂可以方便的分离和循环利用,循环利用7次后,催化活性没有降低,固载催化剂稳定.Using 2-aminobenzaldehyde and NH4 Br/H2 O2 as raw materials, under the catalytic action of 1-methyl-3-(propyltrioxysilane) imidaxole-FeBr4 ionic liquid(FeSIL) supported on SBA-15, the reaction prepare 2-amino-3, 5-divromobenzaldehyde. The ionic liquid catalyst is prepared and screened. The effects of bromide salt type, substrate feed ratio, catalyst dosage, H2 O2 concentration, reaction temperature and reaction time on product yield of are investigated. When the reaction temperature is 40 ℃, the reaction time is 3 h, n(2-amino-benzaldehyde)∶n(NH4 Br)∶n(H2 O2)∶n(FeSIL) = 1∶3∶1.1∶0.03, H2 O2 is 15%, the yield of 2-amino-3, 5-dibromobenzaldehyde reaches98.5% and the content is 99.7%. The supported catalyst can be conveniently separated and recycled. After seven cycles of recycling, the catalytic activity is not reduced, and the solid-supported catalyst is stable.

关 键 词：2-氨基-3 5-二溴苯甲醛 2-氨基苯甲醛 H2O2/NH4Br SBA-15支载离子液体催化剂 溴化反应 

分 类 号：TQ426.94[化学工程]