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博碩士論文 etd-0202110-185640 詳細資訊
Title page for etd-0202110-185640
論文名稱
Title
苯酚膦化物鐵、鋅錯合物之製備及結構鑑定
Preparation and Structural Characterization of Iron and Zinc Complexes Containing a Chelating Phenolato Phosphine Ligand
系所名稱
Department
畢業學年期
Year, semester
語文別
Language
學位類別
Degree
頁數
Number of pages
265
研究生
Author
指導教授
Advisor
召集委員
Convenor
口試委員
Advisory Committee
口試日期
Date of Exam
2009-12-03
繳交日期
Date of Submission
2010-02-02
關鍵字
Keywords
鋅、鐵、苯酚膦化物
Phenolato Phosphine Ligand, Zinc, Iron
統計
Statistics
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中文摘要
我們利用實驗室先前所合成的(Ph-OPO)Na2•(DME)2的化合物作為ligand,分別與一當量和0.5當量的FeCl2反應,都順利合成出兩個順磁性錯合物,也分別做了Evans method和SQUID的實驗,分別對其液態和固態做磁性上的測量,並且也進一步加以討論其磁性現象。
接著我們將原有的H2(Ph-OPO),做進一步的設計,把在donor atom磷上的取代基,由phenyl改為tert-butyl,得到一新的雙苯酚磷化物2,2’-tert-butylphosphinobis(4,6-di-tert-butylphenolate) [(tBu-OPO)2-],嘗試藉由取代基不同的立體障礙與陰電效應,希望能夠得到不同結果,並且拿H2(Ph-OPO)與H2(tBu-OPO),跟一系列鋅(Zn)金屬化合物的反應,利用X-ray及不同核種的NMR鑑定其組成。
Abstract
none
目次 Table of Contents
苯酚膦化物鐵、鋅錯合物
壹、緒論..................................................................................................................1
貳、結果與討論......................................................................................................4
1. [(Ph-OPO)Fe]2·(THF)2的合成與鑑定......................................................4
2. (Ph-OPOH)2Fe·(THF)2的合成與鑑定.....................................................14
3. Zn(tBu-OPOLi)2·(THF)2的合成與鑑定…………………………..……20
4. Zn(tBu-OPOH)2·CH3CN的合成與鑑定..................................................26
5. Zn(Ph-OPOH)2的合成與鑑定.................................................................31
6. Zn2(tBu-OPO)2·THF的合成與鑑定........................................................33
7. Zn2(Ph-OPO)2·(THF)2的合成與鑑定......................................................40
參、結論................................................................................................................46
肆、實驗部分........................................................................................................37
一、一般程序............................................................................. ................49
二、儀器........................................................................................................49
三、實驗步驟................................................................................................50
1. 合成2-bromo-4,6-di-tert-butyl-phenol (HYS1-200) .....................51
2. 合成 (Ph-OPO)H2 (HYS1-155)......................................................51
3. 合成(Ph-OPO)Na2·(DME)2 (HYS1-107) .......................................51
4. 合成H2(tBu-OPO) (HYS2-228) ...................................................52
5. 合成[(Ph-OPO)Fe]2·(THF)2 (HYS1-221) ......................................52
6. 合成(Ph-OPOH)2Fe·(THF)2 (HYS2-245) ......................................53
7. 合成Zn(tBu-OPOLi)2·(THF)2 (HYS2-206) …...............................53
8. 合成Zn(tBu-OPOH)2·CH3CN (HYS2-202)....................................54
9. 合成Zn(Ph-OPOH)2 (HYS2-252、253) .........................................55
10. 合成Zn2(tBu-OPO)2·THF (HYS2-223) .........................................56
11. 合成Zn2(Ph-OPO)2·(THF)2 (HYS2-251) ......................................57
伍、參考文獻........................................................................................................58
參考文獻 References
參考文獻
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