摘要
以2-氯吡啶(1)、2-甲氨基乙醇(2)和4-氟苯甲醛(4)为主要原料,经2步反应合成了4-{2-[N-甲基-N-(2-吡啶基)氨基乙氧基]}苯甲醛(5)。第1步反应n(2)∶n(1)=4∶1,反应温度160℃,反应时间约6 h,采用减压蒸馏进行后处理,2-[N-甲基-N-(2-吡啶基)氨基]乙醇(3)的收率在93%以上,过量2的回收率在97%以上,回收的2可以重复使用。第2步反应用氢氧化钠做碱性试剂,用甲苯和水分别做为两相的溶剂,在相转移催化剂CTAB作用下进行,经优化后5的收率可达90%以上。2步反应总收率达83%以上。
4-{2-[N-Methyl-N-(2-pyridyl)]aminoethoxy}benzaldehyde(5)was synthesized by a two-steps process with 2-chloropyr-idine(1),2-(methylamino)ethanol(2),and 4-fluorobenzaldehyde(4)as principal raw materials.In first step of the process,the mole ratio of 2 to 1 was 4:1,reaction temperature 160℃,reaction time about 6 h,and adopted vacuum distillation in work-up proce-dure.Under such conditions,the yield of 2-[N-methyl-N-(2-pyridyl)amino]ethanol(3)was more than 93%,the rate of recovery of the excess 2 was more than 97%,and recovered 2 could be cyclically used.The second step of process was carried out with sodium hydroxide as basic reagent,toluene and water as solvent of two phases respectively,CTAB as phase-transfer catalyst,gave 5 in more than 90%yield under optimal conditions.The above two steps gave 5 in more than 83%overall yield.
作者
秦丙昌
张高宾
李俊成
靳晓宁
QIN Bin—chang;ZHANG Gao—bin;LI Jun—cheng;JIN Xiao—ning(College of Chemistry and Chemical Engineering,Anyang Normal University,Anyang 455002,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2012年第4期569-573,共5页
Chemical Research and Application
基金
安阳市2010年科技发展计划项目(10043)资助
