摘要
用N-溴代丁二酰亚胺(NBS)作溴化剂,以2,5-二甲基对苯二甲腈为原料,合成了目标化合物2,5-二溴甲基对苯二甲腈。用正交设计实验对影响2,5-二甲基对苯二甲腈生成2,5-二溴甲基对苯二甲腈的溴代反应条件进行了考察,最佳反应条件为:n(2,5-二甲基对苯二甲腈)∶n(NBS)=1∶2.1,反应温度80℃,2,5-二甲基对苯二甲腈浓度0.1 mol/L,反应时间16 h,产率可达31.4%。溴代粗品经反相柱色谱分离〔洗脱液:V(甲醇)∶V(水)=70∶30〕,洗脱组分分别是2-甲基-5-溴甲基对苯二甲腈、2,5-二溴甲基对苯二甲腈、2-甲基-5-(1,1-二溴)甲基对苯二甲腈与2-溴甲基-5-(1,1-二溴)甲基对苯二甲腈。
2,5-Bis （ bromomethyl ） terephthalonitrile was synthesized from 2,5-dimethylterephthalonitrile （RM） using N-bromosuccinimide （NBS） as brominating agent, and products of the α-bromination reaction of 2,5-dimethyherephthalonitrile were characterized. The optimum reaction conditions were n （RM） ： n （ NBS ） = 1 ： 2. 1, concentration of RM in CCl4 0. 1mol/L, reaction temperature 80 ℃ and reaction time 16 h. The reaction mixture of bromination was purified by column chromatography on C18 - RP absorbent [ V（ CH3OH ） ： V（ H20 ） = 70 ： 30 as eluting reagent ] to afford 2-bromomethyl-5- methyherephthalonitrile, 2, 5-bis （bromomethyl） terephthalonitrile, 2-（ dibromomethyl ）-5- methylterephthalonitrile and 2-bromomethyl-5-（ dibromomethyl ） terephthalonitrile sequentially. These four compounds were characterized by means of MS and NMR. Yield of 2,5-bis （bromomethyl） terephthalonitrile was 31.4%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2007年第3期231-234,共4页
Fine Chemicals
