新型Salen催化劑的合成及其在水解動力學拆分中的應用

制藥工程論文編號:ZY048    論文字數:11266,頁數:34

目  錄
 中文摘要 I
 英文摘要 II
 目錄 III
 1. 緒論 1
 1.1 引言 1
 1.2 研究現狀  1
 1.3 論文研究內容 7
 2. 實驗部分 8
 2.1 實驗儀器與試劑 8
 2.2 催化劑合成 9
 2.3 水解動力學拆分環氧氯丙烷 14
3. 結果與討論 15
 3.1 水解動力學拆分條件的優化  15
 3.2 催化劑的回收 18
 4．總結與展望 19
 4.1 總結 19
 4.2 展望 19
 致謝 20
 參考文獻 21
 附錄 23

摘 要：手性環氧氯丙烷是一種極有價值的藥物中間體，本文通過比較文獻報道的幾種方法，選取了水解動力學拆分法制備手性環氧氯丙烷。文中通過逐步嫁接的方法合成了殼聚糖固載的 (Salen)Co(Ⅲ)(OAc)催化劑，并建立了快速可靠的氣相色譜法來跟蹤檢測產物(S)-環氧氯丙烷的對映體過量值（e.e.）。對反應條件進行單因素優化，發現反應在溫度20℃，水用量為0.55當量，催化劑濃度為0.5mol%時，能夠在10小時內得到對映體過量值>99%的(S)-環氧氯丙烷。
 
 關鍵詞：手性環氧氯丙烷；水解動力學拆分；Salen催化劑 
 
 
Abstract: Chiral epichlorohydrin is a very important synton in organic synthesis. The hydrolytic kinetic resolution(HKR) of epichlorohydrin was chosed by compared with many methods reported. The Chitosan supported (Salen)Co(Ⅲ)(OAc) catalyst was synthesized via a stepwise and the enantiomeric excess of the (S)-epichlorohydrin was determined by GC analysis. Optimization of the conditions were investigated by the mono-factor’s experiment. Under the condition that the temperature was 20℃, the water was 0.55 equivalent, and the concentration of the catalyst was 0.5mol%, the enantiomeric excess (e.e.)of the (S)-epichlorohydrin was reach 99% within 10 hours .
 
Keywords：chiral epichlorohydrin; hydrolytic kinetic resolution(HKR);Salen catalyst