二茂铁叔胺化合物毕业论文.docVIP

二茂铁叔胺化合物毕业论文 二茂铁叔胺化合物的环靶化反应及其电化学性能研究 专业 ： 化学与化工 摘 要 二茂铁三氯氧磷、反应生成甲酰基二茂铁甲酰基二茂铁与盐酸羟胺碳酸氢钠在溶剂缩合成甲酰基二茂铁肟；甲酰基二茂铁肟氢化铝锂溶剂四氢呋喃成二茂铁甲基胺 二茂铁甲基胺苯甲醛2，6-二氯苯甲醛无水甲醇成相应希夫碱，希夫碱甲基化得到叔胺，叔胺 通过红外光谱和核磁共振测定希夫碱甲基化 关键词 二茂铁/希夫碱/ SYNTHESIS OF FERROCENE METHYLAMINEPALLADACYCLES COMPOUNDS ABSTRACT 1.The formyl ferrocene 1 was synthesizend by the condensation of the ferrocene and phosphorus oxychloride, N, N-dimethylformamide, which reacted with hydroxylamine hydrochloride in the presence of sodium bicarbonate in methanol producing the formyl ferrocene oxime 2. The ferrocene oxime 2 was reduced by lithium aluminium hydride in dry tetrahydrofuran giving the ferrocene methylamine 3 , which were confirmed by infrared spectroscopy. 2.The four Schiff bases（4a、4b、4c、4d） were synthesized by formyl ferrocene amine, Furfural, thiophene formaldehyde（benzaldehyde 、2,6 – Dichlorobenzaldehyde) in anhydrous methanol, respectively. Which were dealed with formaldehyde and reduced by sodium borohydride in methanol producing the ferrocenyl tertiary amine. The ferrocenyl tertiary amine were reacted with Li2PdCl4 in anhydrous methanol giving the dimer cyclopalladated compound, which were reacted with triphenylphosphine resulting in the monomer cyclopalaldated compound. 3. By infraring redients spectroscopy and nuclear magnetic resonance to measured the structure of compounds and by infraring cyclic voltammetry to measured the performance of compounds . KEYWORDS ferrocene, schiff base, N methylation, palladium-based 目 录 摘 要 I ABSTRACT II 1 引言 1 2 实验部分 3 2.1 实验仪器 3 2.2 实验药品及试剂 4 2.3 溶液和洗液的配制 5 2.3.1羧甲基纤维素钠溶液的配制 5 2.3.2铬酸洗液的配制 5 2.3.3四丁基高氯酸铵（TBAP）的制备 2.4 薄层色谱板的制备 6 2.4.1 铺板 6 2.4.2 薄层板的活化 6 2.4.3 点样 6 2.4.4 展开剂的选择 6 2.4.5 展开 7 2.4.6 产物的分离 7 2.5柱色谱的制备 7 2.5.1 装柱子 7 2.5.2 分离产物 7 2.5.3 后处理 7 2.6 实验所用溶剂的纯化 8 2.6.1 工业用无水二氯甲烷的制备 8 2.6.2 无水甲醇的制备 8 2.6.3 无水四氢呋喃的制备 9 2.7 实验过程 10 2.7.1 甲酰基二茂铁的制备 10 2.7.2 甲酰基二茂铁肟的制备 10 2.7.3 二茂铁甲基胺的制备 11 2.7.4 希夫碱的合成及还原 11 2.