摘要
以2-氨基-1-丁醇、多聚甲醛和二氯乙酰氯为原料,氢氧化钠水溶液作缚酸剂,采用“一锅法”简便而高效地合成了标题化合物。通过正交试验设计获得最佳反应条件:甲苯作溶剂,反应温度-3~3℃,搅拌时间3h,2-氨基-1-丁醇与多聚甲醛的物质的量比为1∶1.4,产率为64.37%。产品经红外光谱、核磁共振谱和元素分析进行结构表征。本方法原料廉价易得,反应条件温和、操作简单,为该类化合物的合成提供了一种新的便利途径。
The title compound was synthesized efficiently by one - pot method from 2 - Amino - 1 - butanol, paraformaldehyde,dichloroacetyl chloride,and sodium hydroxide solution was used as an acid binding agent. By orthogonal experimental design method,the optimum conditions were obtained as following:toluene was used as solvent,the rection temperature was - 3 ~ 3℃ ,stirring time was 3h,the molar ratio of 2 - amino - 1 - butanol to paraformaldehyde was 1:1. 4, the yield was 64. 37% . The products were charactered by infrared spectrum(IR),nuclear magnetic resonance spectrum (NMR),and elementary analysis. The method might be a new convenient rote for the synthesis of compounds for its adventiages of simple operation,mild conditions and the raw materials are easy to obtain.
出处
《山东化工》
CAS
2014年第7期13-14,18,共3页
Shandong Chemical Industry
基金
黑龙江省教育科学"十二五"规划2012年度课题(青年专项课题):药学专业有机化学实验创新教学体系研究(GBD1212075)
关键词
二氯乙酰基噁唑烷
一锅合成法
表征
dichloroacetyl oxazolidine
one pot synthesis
characterization