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作 者:何玉晖[1] 羊衍秋[1] 杨亮[1] 张晗[2] 罗顺忠[1]
机构地区:[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
出 处:《化学研究与应用》2013年第6期875-879,共5页Chemical Research and Application
基 金:国家自然科学基金重大研究计划培育项目(No.91026022)资助
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-(ω-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∶C3Br2∶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α,ω-二溴烷烃的烷基链长度增加而降低。Derivation of calixarenes on the upper/lower rims with ligands was the main route to improve their eomplexation and se- lective capabilities for separating actinides and lanthanides. N-(w-bromoalkyl)phthalimide was an important intermediate in the synthesis process of ca]ixarene derivatives. In this article, using N-(ω-bromoalkyl) phthalimide as the template, the relation between the yield of N-(ω-bromoalky]) phthalimide and reaction conditions were investigated. The yield of N-(ta-bromoalkyl) phthalimide was above 92% through optimizing the reaction conditions. The type of the phase transfer catalysts and their amounts and the a- mounts of K2CO3 were the key influence factors in the N-alkylation of phthalimide reaction by the solvent-free way. In addition ,the increasing of the length of chains would decrease the yield of N-(ω-bromoalkyl)phthalimide under the same reaction conditions.
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