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研究生:黃家榆
研究生(外文):JiaYu HUANG
論文名稱:末端含鹵素短氟鏈聯吡啶接上鈀、鉑金屬錯合物之相關研究
論文名稱(外文):Synthesis, Characterization and Studies of Pd and Pt Complexes with Short Fluoro-ponytailed Bipyridine Ligands Possessing Terminal Halogen
指導教授:呂良賜
口試委員:芮祥鵬劉陵崗江志強
口試日期:2016-07-29
學位類別:碩士
校院名稱:國立臺北科技大學
系所名稱:有機高分子研究所
學門:工程學門
學類:化學工程學類
論文種類:學術論文
畢業學年度:104
語文別:中文
中文關鍵詞:X-射線衍射鹵素鍵金屬錯合物短氟鏈聯吡啶螯合劑
外文關鍵詞:X-rayHalogen bondMetal complexPlatinumPalladiumFluorous Bipyridine ligands
相關次數:
  • 被引用被引用:3
  • 點閱點閱:38
  • 評分評分:
  • 下載下載:2
  • 收藏至我的研究室書目清單書目收藏:0
本實驗室多年前即致力於對氟化物研究,合成之短氟鏈聯吡啶螯合劑,目前合成產率平均可達85~95%,利用GC-MS測定,純度可達99.9%,而這次實驗將氟鏈末端改為氯原子[4,4′-bis(RfCH2OCH2)-2,2′bipyridine和5,5′-bis(RfCH2OCH2)-2,2′bipyridine,Rf = CF2CF2Cl],與以往氟鏈末端為氫或氟原子不同,將合成出的螯合劑接上鈀、鉑金屬錯合物[PtX2(4,4′-bis(RfCH2OCH2)-2,2′bipyridine)、PdX2(4,4′-bis(RfCH2OCH2)-2,2′bipyridine)和PtX2(5,5′-bis(RfCH2OCH2)-2,2′bipyridine)、PdX2(5,5′-bis(RfCH2OCH2)-2,2′bipyridine),Rf = CF2CF2Cl,X=Cl、Br、I],利用雙溶劑法,控制析出速率、溫度…等變因,並使用NMR(1H、13C、19F)、FT-IR、高解析質譜儀、X-ray單晶繞射儀及熔點測定儀來探討其結構及性質,發現同一金屬錯合物於不同條件養出之晶體,可得不同晶體結構,其分子間堆疊也不盡相同,而氟鏈末端為氯之金屬錯合物則形成分子間鹵素鍵與其碳-氯鍵長改變。
附錄:利用銅催化法取代金屬錯合物上之鹵素。
Years ago our Lab started to synthesize polyfluorinated compounds and promoted their recognition considerably. On continuation of our prior studies, I synthesized Bipyridine ligands having terminal Halogen and its palladium/platinum metal complex in this research to study their structural properties. Ligands [4,4′-bis(RfCH2OCH2)-2,2′bipyridine, 5,5′-bis(RfCH2OCH2)-2,2′bipyridine [Rf = CF2CF2Cl] were synthesized with the average yield of 85~95%. The purity of the ligand is close to 99.9%.
The newly synthesized ligands were treated with Palladium and Platinum Metals to generate their corresponding Metal complex. The synthesized ligand and their metal complex have been characterized using IR, NMR, HR-FAB, Single Crystal X-ray diffraction, and Melting point techniques. We have attempted to prepare crystals with various structures, using dual solvent and change of temperature during recrystallization.
Appendix:Using copper catalysis to replace halogen attached on metal complex.
目 錄
中文摘要 i
英文摘要 ii
誌謝 iii
目錄 iv
表目錄 v
圖目錄 vi
縮寫對照表 ...xvii
第一章 緒論 - 1 -
1-1 前言 - 1 -
1-2相關理論與文獻回顧 - 2 -
1-2-1 聯吡啶 - 2 -
1-2-2 鹵素鍵 - 3 -
1-2-3 藍位移氫鍵 - 5 -
第二章 實驗方法 - 6 -
2-1藥品材料 - 6 -
2-2儀器 - 7 -
2-3實驗部分 - 8 -
2-3-1合成螯合劑 - 8 -
2-3-2合成金屬錯合物 - 10 -
2-3-3 再結晶 - 11 -
2-3-4螯合劑和鈀、鉑金屬錯合物之鑑定數據 - 12 -
第三章 結果與討論 - 62 -
3-1儀器鑑定 - 62 -
3-2 晶體結構探討 - 65 -
3-2-1氟鏈末端含氫、氟之金屬錯合物 - 65 -
3-2-2 氟鏈末端含氯之金屬錯合物 - 69 -
第四章 結論 - 81 -
圖譜 - 82 -
參考文獻 - 151 -
附錄A 晶體結構 - 154 -
附錄B 利用銅催化法合成含氟鏈鉑金屬錯合物 - 160 -
參考文獻
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