双乙酰基二茂铁的合成及其与1,10-邻菲啰啉之间的光配体交换反应产物剖析--推荐一个新颖有趣的综合化学实验  

Synthesis of Diacetylferrocene and Analysis of Photo-ligand Exchange Reaction Product between Diacetylferrocene and 1,10-Phenanthroline:A New and Interesting Comprehensive Chemistry Experiment

作　　者：孟祥茹[1] 李纲[1] Xiangru Meng;Gang Li(Green Catalysis Center,College of Chemistry,Zhengzhou University,Zhengzhou 450001,China.)

机构地区：[1]郑州大学化学学院,绿色催化中心,郑州450001

出　　处：《大学化学》2021年第6期154-159,共6页University Chemistry

基　　金：2017年郑州大学校级质量工程项目“重点教材建设项目”。

摘　　要：首先以二茂铁和乙酰氯为原料,通过Friedel-Crafts酰基化反应制备1,1’-二乙酰基二茂铁(DAF),此过程涉及低温控制、无水无氧操作、萃取、减压蒸馏、重结晶等基本操作;然后利用DAF的光敏性以及1,10-邻菲啰啉(phen)的强螯合能力,在可见光的照射下进行配体交换反应:phen取代乙酰基环戊二烯配体并得到配合物[Fe(phen)_(3)](C_(5)H4COCH_(3))_(2)·CH_(3)CN·2H_(2)O。最后借助粉末X射线衍射、元素分析、红外光谱、核磁共振氢谱等手段确定光反应产物的组成。本实验难度适中,测试手段多样,使得大三或者大四的本科生能够在综合化学实验(I)以及无机、分析、有机化学实验的基础上,独立完成一个基本的科研训练过程。1,1-diacetylferrocene(DAF)was synthesized through Friedel-Crafts acylation reaction by using ferrocene and acetylchloride as starting materials.This process involves basic laboratory skills,such as low temperature control,anhydrous and anoxic operation,extraction,vacuum distillation and recrystallization.The photo-ligand exchange reaction between DAF and 1,10-phenanthroline(phen)was carried out under visible light irradiation due to the photosensitivity of DAF and the strong chelating ability of phen.Phen substituted acetyl cyclopentadiene ligand,and produced complex[Fe(phen)_(3)](C_(5)H4COCH_(3))_(2)·CH_(3)CN·2H_(2)O.The composition of the photoreaction product was determined by means of powder X-ray diffraction,elemental analysis,infrared spectrum and 1H NMR spectra.This comprehensive chemistry experiment is appropriate in difficulty,and the testing methods are diversified,which enables junior or senior undergraduates to complete a basic scientific research training process independently on the basis of comprehensive laboratory(I)and basic inorganic,analytical and organic chemistry laboratories.

关 键 词：1 1’-二乙酰基二茂铁 1 10-邻菲啰啉 光配体交换反应 综合化学实验 

分 类 号：G64[文化科学—高等教育学] O6[文化科学—教育学]