摘要
以5-甲氧基吲哚为原料,经加热反应、真空去挥发物、碱液稀释调和、溶剂萃取、减压蒸馏等工艺过程制得5-甲氧基-3-(2-二异丙基氨基乙基)-吲哚,研究了反应时间、反应温度、溶剂、原料的配比等因素对收率的影响.获得了较佳的合成工艺条件,即反应时间为18~19h,反应温度为130~140℃,用环丁砜作溶剂,反应原料配比(质量比)为m(5-甲氧基吲哚)∶m(DIPEA)∶m(碘代异丙烷)=1∶2.73∶3.57时,收率可达70%.
The experiment has studied the technological process by which 5-methoxy-indole was heated,evaporated under vacuum,diluted by lye,extracted by solvent,distilled under vacuum and so on for making (5-methoxy-3-)(2-disopropy amidogenl ethyl)-indole.Factors which may affect the yield of reaction,such as reaction time,reaction temperature,solvent,material quantity are discussed.Under these process conditions:(reaction) temperature is 130~140 ℃,reaction time is 18~19 h,material quantity is (5-methoxy-indole)∶(DIPEA)∶(2-Iodopropane)=1∶2.73∶3.57.Solvent is cyclobutylsulfone,the yield can reach 70%.
出处
《南昌大学学报(工科版)》
CAS
2003年第3期66-69,共4页
Journal of Nanchang University(Engineering & Technology)