相转移催化无溶剂合成N-(ω-溴烷基)邻苯二甲酰亚胺.pdf

第25卷第6期
化学研究与应用
Vol 25. No 6
2013年6月
Chemical Research and Application
文章编号:1004-1656(2013)06-0875-05
相转移催化无溶剂合成N-(の-溴烷基)
邻苯二甲酰亚胺
何玉晖,羊衍秋,杨亮,张晗2,罗顺忠
(1.中国工程物理研究院核物理与化学研究所,四川绵阳621900;
2.西南科技大学环境与资源学院,四川绵阳621000
摘要:本文以N-(3-溴丙基)邻苯二甲酰亚胺合成为模板反应,研究了相转移催化无溶剂合成N-(-溴烷基)
邻苯二甲酰亚胺的影响因素,实验证实相转移催化剂及其用量、催化剂K2CO3的用量等对反应的影响明显,
得到N-(3-溴丙基)邻苯二甲酰亚胺的优化合成条件为:反应物配比为PA:CgBr2:K2CO3:TBAB=1:2:4:0.2
反应温度80℃,反应时间1h,N-(3-溴丙基)邻苯二甲酰亚胺产率为92%。在相同反应条件下,N-(ω-溴烷基)
邻苯二甲酰亚胺的产率随a,-二溴烷烃的烷基链长度增加而降低。
关键词:邻苯二甲酰亚胺;-烷基化;相转移催化剂;无溶剂有机合成
中图分类号:0623.62文献标志码:A
Solvent-free synthesis of N-(A-bromoalkyl )phthalimide
using phase transfer catalysts
HE Yu-hui, YANG Yan-qiu YANG Liang ZHANG H LUO Shun-nog
(1. Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900, China
2. College of Environment and Resources, South-west University of Science and Technology, Mianyang 621000, China)
Abstract: Derivation of alixarenes on the upper/lower ms with igands was the main route to improve their complexation and e-
lective capabilities for separating actinides and lanthanides. N-(A-brmalkyl )phthalimide was an important intermediate in the
synthesis process of calixarene derivatives. In this article, using -(A-bromoalk l)phthalimide as the template, the relation between
the yield of -(a-bromoalk l )phthalimide and reaction conditions were investigated. The yield of N-(A-bromoalkyl)phthalimide
was above 92% through optimizing the reaction conditions. The type of the phase transfer catalysts and their amounts and the a-
mounts ofk C0; were the key influence factors in the N-alk lation of phthalimide reaction by the solvent-free way. In addition, the
increasing of the length of chains would decrease the yield of N-(A-romoalkyl )phthalimide under the same reaction conditions
Key words: phthal mide N-alkylation; phase transfer catalyst solvent-free organic synthesis
以杯芳烃为骨架,在上/下缘链接氨基甲酰甲基其与钢系元素间的分离因子。杯芳烃上/下缘配位
氧化隣(CMPO)呲啶酰胺等对锕系元素选择性配位基团衍生化的主要合成路线为利用M-(ω-溴烷基)邻
基团,提高配位基的预组织性,能提高锕系萃取率及苯二甲酰亚胺在NaH作用下与酚羟基醚化后用肼
收稿日期:201212-18;修回日期:2013-02-28
甚金项目:国家自然科学基金重大研究计划培育项目(Na.9102602)资助
联系人简介:罗顺忠(1955-),男,研究员,主要从事放射性核素分离研究。E-mai:luoshan(@caep.ac.cn