综合化学实验中空气敏感合成实验的选取和教学
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摘要
选择"硅基芳胺的合成与表征"作为综合化学实验"无水无氧合成技术"的教学内容,实验涉及特殊用途玻璃仪器的干燥与组装、空气敏感物质的操作、惰性气体保护下的化学反应、溶剂浓缩、萃取、少量液体的减压蒸馏以及结构测定等操作。深入分析了无水无氧反应装置的准备、溶剂和物料的转移、正丁基锂的取用、双排管和施伦克玻璃仪器的使用等操作细节问题,并对产物的核磁共振氢谱进行了解析。通过该实验,学生能够实践较高层次的化学实验操作,对拓宽学生专业知识面、提高学生综合实验操作技能有良好的教学效果。
"Synthesis and characterization of an aryl silylamine" was selected as the teaching content of "Schlenk line technique", which involves drying and assembly of glass instruments for special purposes, operation of air sensitive substances, reactions under inert gas protection, solvent concentration, extraction, distillation under reduced pressure, and molecular structure determination. In this article, the following experimental operations were discussed in detail, including the preparation of experimental devices, the transfer of solvents and reactants, a special method of transferring n-butyllithium, operations of Schlenk line, Schlenk flasks and water-free solvent flasks. The hydrogen spectra of nuclear magnetic resonance(NMR) of the aryl silylamine were analyzed. This experiment enables students to practice the experimental operations at the higher levels. This could have a good teaching effect, in broadening students' professional knowledge and improving their operating skills in comprehensive chemical experiment.
"Synthesis and characterization of an aryl silylamine" was selected as the teaching content of "Schlenk line technique", which involves drying and assembly of glass instruments for special purposes, operation of air sensitive substances, reactions under inert gas protection, solvent concentration, extraction, distillation under reduced pressure, and molecular structure determination. In this article, the following experimental operations were discussed in detail, including the preparation of experimental devices, the transfer of solvents and reactants, a special method of transferring n-butyllithium, operations of Schlenk line, Schlenk flasks and water-free solvent flasks. The hydrogen spectra of nuclear magnetic resonance(NMR) of the aryl silylamine were analyzed. This experiment enables students to practice the experimental operations at the higher levels. This could have a good teaching effect, in broadening students' professional knowledge and improving their operating skills in comprehensive chemical experiment.
引文
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[2]有机合成实验室手册.第22版.万均,温永红,陈玉,赵亮,译.北京:化学工业出版社, 2010, 16–29.
[3]薛永强,张蓉.现代有机合成方法与技术.北京:化学工业出版社, 2007.
[4]孙学芹.大学化学, 2011, 26(1), 48.
[5]刘超,李沙沙,陈晴晴,徐丽娟,徐基贵,张克营.宿州学院学报, 2012, 27(1), 117.
[6]李珺,张逢星,李剑利.综合化学实验.北京:科学出版社, 2011, 80–81, 87–89.
[7]何仁,陶晓春,张兆国.金属有机化学.上海:华东理工大学出版社, 2007, 12–19.
[8]Lipschutz, M. I.; Chantarojsiri, T.; Dong, Y.; Tilley, T. D. J. Am. Chem. Soc. 2015, 137, 6366.
[9]Zadrozny, J. M.; Atanasov, M.; Bryan, A. M.; Lin, C. Y.; Rekken, B. D.; Power, P. P.; Neese, F.; Long, J. R. Chem. Sci. 2013, 4, 125.
[10]Chao, Y. W.; Wexler, P. A.; Wigley, D. E. Inorg. Chem. 1989, 28, 3860.
[11]Xu, M. T.; Jupp, A. R.; Stephan, D. W. Angew. Chem. Int. Ed. 2017, 56, 14277.
[12]Schulz, A.; Villinger, A.; Westenkirchner, A. Inorg. Chem. 2013, 52, 11457.
[13]徐如人,庞文琴,霍启升.无机合成与制备化学.第2版.北京:高等教育出版社, 2009, 429–433.