用自制的硫酸氢l-甲基-3.-(3-磺酸基丙基)咪唑([MIMPS]HSO4)酸性离子液体作为水杨酸与醇的酯化反应催化剂,考察了温度、时间、物料配比和离子液体用量等因素对酯化反应的影响,优化的最佳反应条件为:微波辐射时间20 min,反应温度95℃,醇与酸摩尔比3∶1(水杨酸的量为0.02 mol),[MIMPS]HSO4用量10 mmol,水杨酸甲酯的产率和选择性分别为91.9％和99.0％.离子液体回收循环使用4次,催化效率不变.与热催化酯化反应相比,微波辐射可缩短反应时间；水杨酸与不同碳链醇的酯化产率随着碳链的增加而降低,同碳链的伯醇酯化率比仲醇高.
参考文献
| [1] | Peters T A,Benes N E,Holmen A,et al.Comparison of Commercial Solid Acid Catalysts for the Esterification of Acetic Acid with Butanol[J].Appl Catal A:Gen,2006,297(2):182-188. |
| [2] | Schildhauer T J,Hoek I,Kapteijn F,et al.Catalysed Esterification of Hexanoic Acid with 1-Octanol:Kinetics,Side Reactions and the Role of Water[J].Appl Catal A:Gen,2009,358(2):141-145. |
| [3] | LU Zekai,ZHU Wanren.Synthesis of Isopropyl Salicylicate with Solid Ferric Sulphate as a Catalyst[J].Chinese J Org Chem,2002,22(6):450-452(in Chinese).卢泽楷,朱万仁.固体铁系超强酸的制备及催化水杨酸异丙酯的合成[J].有机化学,2002,22(6):450-452. |
| [4] | Bamoharram F F,Heravi M M,Roshani M,et al.Preyssler Catalyst,[NaP5W30O110]14-:A Green,Efficient and Reusable Catalyst for Esterification of Salicylic Acid with Aliphatic and Benzylic Alcohols[J].Appl Catal A:Gen,2006,302(1):42-47. |
| [5] | Jiang D,Liu J,Wang Y Y,et al.The Synthesis of Salicylate Prompted by Br(o)nsted Acidic Ionic Liquids[J].J Chil Chem Soc,2009,54(1):40-42. |
| [6] | Shi H,Zhu W S,Li H M,et al.Microwave-accelerated Esterification of Salicylic Acid Using Br(o)nsted Acidic Ionic Liquids as Catalysts[J].Catal Commun,2010,11(7):588-591. |
| [7] | WANG Qiang,LIANG Hongze,BAO Weiliang.Preparation of Task-Specific Ionic Liquids and Their Application in Organic Synthesis[J].Chinese J Appl Chem,2007,24(2):117-123(in Chinese).王强,梁洪泽,包伟良.功能化离子液体的制备及其在合成中的应用[J].应用化学,2007,24(2):117-123. |
| [8] | Duan Z Y,Gu Y L,Deng Y Q.Neutral Ionic Liquid[BMIm]BF4 Promoted Highly Selective Esterification of Tertiary Alcohols by Acetic Anhydride[J].J Mol Catal A:Chem,2006,246(1/2):70-75. |
| [9] | Major B,Kelemen-Horváth I,Csanádi Z,et al.Microwave Assisted Enzymatic Esterfication of Lactic Acid and Ethanol in Phosphonium Type Ionic Liquids as Co-solvents[J].Green Chem,2009,11:614-616. |
| [10] | FANG Dong,LIU Zuliang,ZHOU Xinli.Catalytic Synthesis of Benzyl Acetate in Task-Specific Room Temperature Ionic Liquid[J].Chinese J Appl Chem,2007,24(1):85-89(Chinese).方东,刘祖亮,周新利.功能化离子液体室温催化合成乙酸苄酯[J].应用化学,2007,24(1):85-89. |
| [11] | Thomazeau C,Olivier-Bourbigou H,Magna L,et al.Determination of An Acidic Scale in Room Temperature Ionic Liquids[J].J Am Chem Soc,2003,125(18):5264-5265. |
| [12] | Gu Y L,Zhang J,Duan Z Y,et al.Pechmann Reaction in Nonchloroaluminate Acidic Ionic Liquids under Solvent-free Conditions[J].Adv Synth Catal,2005,347(4):512-516. |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%