摘要
以二乙氨基乙醇、3,4 二氯氯化苄为原料 ,四丁基溴化铵为相转移催化剂 (PTC) ,氢氧化钠固体为碱 ,苯为溶剂 ,经Williamson醚化反应合成N ,N 二乙基氨基乙基 3,4 二氯苄基醚 ,产率最高可达 84 5 % ,质量分数为 98 7%。最佳合成条件 :n(Et2 NCH2 CH2 OH)∶n(Cl2 ArCH2 Cl)∶n(NaOH)∶n(PTC) =1 2∶1∶2∶0 0 5 ,反应时间为 2h ,反应温度为 6 0℃。产物经过沸点、折光率、红外光谱。
N,N Diethylaminoethyl 3,4 dichlorobenzyl ether was synthesized in good yield(84 5%,high purity of 98 7%) by Williamson reaction of diethylaminoethanol and 3,4 dichlorobenzyl chloride using Bu 4NBr as phase transfer catalyst,sodium hydroxide as base and benzene as solvent.The optimized conditions were as follows.Molar ratio of diethylaminoethanol to 3,4 dichlorobenzyl chloride to sodium hydroxide to Bu 4NBr was 1 2∶1∶2∶0 05,reaction time was 2 h and reaction temperature was 60 ℃.Structure of the product was confirmed by boiling point,refractive index,IR and 1H NMR spectrometry.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2002年第5期304-306,共3页
Fine Chemicals