【正文】 二茂鐵叔胺化合物畢業(yè)論文 I 二茂鐵叔胺化合物畢業(yè)論文 二茂鐵叔胺化合物的環(huán)靶化反應(yīng)及其電化學(xué)性能研究 專業(yè) ： 化學(xué)與化工 二茂鐵叔胺化合物畢業(yè)論文 II 摘 要 1. 二茂鐵 和 三氯氧磷、 DMF 在無水氯仿中 反應(yīng)生成甲酰基二茂鐵 ； 甲酰基二茂鐵與鹽酸羥胺 、 碳酸氫鈉在 無水甲醇 溶劑 中 縮合 生 成甲酰基二茂鐵肟；甲酰基二茂鐵肟 和 氫化鋁鋰 在 溶劑四氫呋喃 中生 成二茂鐵甲基胺 。 2. 二茂鐵甲基胺 分別與糠醛、噻吩甲醛、 苯甲醛 、 2， 6二氯苯甲醛 在 無水甲醇中 生 成 四個 相應(yīng) 的 希夫堿，希夫堿 經(jīng)硼氫化鈉還原得到相對應(yīng)的仲胺化合物，其和甲醛、硼氫化鈉氮 甲基化 反應(yīng) 得到 相應(yīng)的 叔胺，叔胺 與氯化鈀鋰、乙酸鈉在甲醇溶劑中反應(yīng)生成相應(yīng)的二聚體，在二氯甲烷溶劑中二聚體和三苯基膦環(huán)鈀解聚生成相應(yīng)的環(huán)鈀解聚體。 3. 通過紅外光譜和 核磁共振 測定 希夫堿 還原物仲胺、氮 甲基化 產(chǎn)物叔胺、環(huán)鈀解聚物的結(jié)構(gòu)并通過循環(huán)伏安法測定它們的電化學(xué)性能。 關(guān)鍵詞 二茂鐵 /希夫堿 /氮甲基化 /環(huán)鈀化 二茂鐵叔胺化合物畢業(yè)論文 III SYNTHESIS OF FERROCENE METHYLAMINEPALLADACYCLES COMPOUNDS ABSTRACT formyl ferrocene 1 was synthesizend by the condensation of the ferrocene and phosphorus oxychloride, N, N39。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. 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 pound, which were reacted with triphenylphosphine resulting in the monomer cyclopalaldated pound. 3. By infraring redients spectroscopy and nuclear magic resonance to measured the structure of pounds and by infraring cyclic voltammetry to measured the performance of pounds . KEYWORDS ferrocene, schiff base, N methylation, palladiumbased 二茂鐵叔胺化合物畢業(yè)論文 IV 目 錄 摘 要 .................................................................................................................................II ABSTRACT........................................................................................................................... III 1 引 言 .................................................................................................................................. I 2 實驗部分 ........................................................................................................................ 1 實驗儀器 ............................................................................................................ 1 實驗藥品及試劑 .............................................................................................. 2 溶液和 洗液的配制 .......................................................................................... 3 羧甲基纖維素鈉溶液的配制 ...................................................................... 3 鉻酸洗液的配制 .......................................................................................... 3 四丁基高氯酸銨（ TBAP）的制備 薄層色譜板的制備 .......................................................................................... 3 鋪板 ............................................................................................................. 3 薄層板的活化 ............................................................................................. 4 點樣 ............................................................................................................. 4 展開劑的選擇 ............................................................................................. 4 展開 ............................................................................................................. 4 產(chǎn)物的分離 ................................................................................................. 5 柱色譜的制備 .................................................................................................... 5 裝柱子 ......................................................................................................... 5 分離產(chǎn)物 ..................................................................................................... 5 后處理 ......................................................................................................... 5 實驗所用溶劑的純化 ..................................................................................... 5 工業(yè)用 無水二氯甲烷的制備 ..................................................................... 5 無水甲醇的制備 ......................................................................................... 6 無水四氫呋喃的制備 ................................................................................. 6 實驗過程 ............................................................................................................ 7 甲?；F的制備 ................................................................................. 7 甲酰基二茂鐵肟的制備 ............................................................................. 8 二茂鐵甲基胺的制備 ................................................................................. 8 希夫堿的合成 及還原 ................................................................................. 9 二茂鐵叔胺化合物畢業(yè)論文 V 仲胺的氮甲基化 ........................................................................................10 環(huán)鈀化反應(yīng) ................................................................................................10 3 產(chǎn) 物 結(jié) 構(gòu) 的 測 定 及 電 化 學(xué) 性 能 研究 .............................................. 核磁共振測定結(jié)構(gòu) .......................................... 循環(huán)伏安法測定電化學(xué)性能 .................................. 紅外光譜測定結(jié)構(gòu) .......................................... 4 結(jié)果與討論 ..................................................................................................................21 反應(yīng)的