Claisen縮合合成三氟乙酰乙酸乙酯

制藥工程論文編號:ZY114    論文字?jǐn)?shù):9207,頁數(shù):22

 目  錄
中文摘要...............................................................Ⅰ
英文摘要...............................................................Ⅱ
目錄...................................................................Ⅲ
1.緒論.................................................................1
   1.1 前言............................................................1
 1.2 研究現(xiàn)狀........................................................2
      1.2.1以氫化鈉作為催化劑.........................................2
      1.2.2以金屬鈉作催化劑...........................................2
      1.2.3以乙醇鈉為催化劑...........................................2
 1.3 實驗設(shè)計........................................................4
2.實驗部分.............................................................5
 2.1 實驗材料........................................................5
       2.1.1 實驗試劑..................................................5
       2.1.2 實驗儀器..................................................5
 2.2 反應(yīng)原理........................................................6
 2.3 實驗步驟........................................................6
       2.3.1 縮合......................................................6
       2.3.2 中和......................................................7
       2.3.3 乙酰化....................................................7
        2.3.4 分離純化..................................................7
3.結(jié)果與討論...........................................................8
   3.1 對縮合過程中各因素的探討........................................8
       3.1.1不同催化劑對收率的影響.....................................8
       3.1.2不同催化劑量對收率的影響...................................8
       3.1.3不同溶劑對收率的影響.......................................9
       3.1.4 不同反應(yīng)時間對收率的影響..................................10
 3.2 對中和過程中各因素的探討........................................10
3.2.1不同酸對收率的影響........................................10
 3.3 對乙酰化過程各因素的探討........................................11
3.3.1 不同乙酰氯量對收率的影響..................................11
 3.4 產(chǎn)物的表征......................................................12
 4.總結(jié)與展望............................................................15
 致謝....................................................................17
 參考文獻................................................................18

摘 要： 三氟乙酰乙酸乙酯是合成氟雜環(huán)醫(yī)藥和農(nóng)藥的中間體。本文闡述了以三氟乙酸乙酯和乙酸乙酯為原料，在堿性催化劑下進行Claisen縮合，并用質(zhì)子酸進行中和，乙酰化等步驟合成三氟乙酰乙酸乙酯的方法。對合成三氟乙酰乙酸乙酯的反應(yīng)條件進行了優(yōu)化探討，結(jié)果表明實驗的最佳反應(yīng)條件為：以環(huán)己烷為溶劑，1.2當(dāng)量的金屬鈉為催化劑，反應(yīng)物摩爾比為1：1.5，縮合反應(yīng)時間為4小時，甲酸中和，以1當(dāng)量的乙酰氯進行乙酰化，最后得到的收率為78%。
關(guān)鍵字：三氟乙酰乙酸乙酯；Claisen縮合; 乙酰化

Abstract: Ethyl-trifluoroacetoacetate is used as important intermediate in the synthesis of pharmaceutical or plant protection industry. This paper describe a way of preparation of  ethyl-trifluoroacetoacetate  by  following steps . In the first step, ethyl-trifluoroacetate condensed with ethyl acetate in the presence of alkaline catalyst. The follow steps are neutralization and acetylation, then optimize the reaction conditions of the preparation of  ethyl-trifluoroacetoacetate.  The study show that the optimal reaction conditions as following: cyclohexane as solvent, 1.2 equivalent of sodium for catalyst, reactant molar ratio is 1 : 1.5, condensation reaction for 4 hours, formic acid for neutralization and 1 equivalent of chloride for acetylation, the yield of ethyl-trifluoroacetoacetate is 78%.

Keywords:  Ehyltrifluoroacetoacetate;；Claisen condensation；Acetylation