二茂鐵叔胺化合物的環(huán)靶化反應及其電化學性能研究.doc
二茂鐵叔胺化合物的環(huán)靶化反應及其電化學性能研究,摘 要1.二茂鐵和三氯氧磷、dmf在無水氯仿中反應生成甲酰基二茂鐵;甲?;F與鹽酸羥胺、碳酸氫鈉在無水甲醇溶劑中縮合生成甲?;F肟;甲?;F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...
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摘 要
1. 二茂鐵和三氯氧磷、DMF在無水氯仿中反應生成甲?;F;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的希夫堿,希夫堿經(jīng)硼氫化鈉還原得到相對應的仲胺化合物,其和甲醛、硼氫化鈉氮甲基化反應得到相應的叔胺,叔胺與氯化鈀鋰、乙酸鈉在甲醇溶劑中反應生成相應的二聚體,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性能。
關(guān)鍵詞 二茂鐵/希夫堿/氮甲基化/環(huán)鈀化
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