相转移催化无溶剂合成N-(ω-溴烷基)邻苯二甲酰亚胺

Solvent-free synthesis of N-(ω-bromoalkyl) phthalimide using phase transfer catalysts

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.