将三丁基氯化锡与SBA-15介孔分子筛在N2气气氛中进行回流反应,得到有机锡无机配合物(C4H9)3Sn-O-SBA-15[Bu3SnS].利用X射线衍射(XRD)、透射电子显微镜(TEM)、氮气吸附脱附、固体核磁(NMR)和吡啶吸附脱附红外光谱分析(Py-IR)等方法对产物的组成、结构和性质进行了表征.结果表明,产物Bu3 SnS具有高度有序的六方介孔结构,与SBA-15相比,Bu3 SnS比表面积、孔容和孔径变小,酸性增强.Bu3 SnS对苯甲醚Friedel-Crafts酰基化反应具有优异的催化性能,当反应温度为130℃,n(苯甲醚)∶n(苯甲酰氯)=1.0∶2.0,w(cat) =6％(相对于苯甲醚用量),反应时间为5h,苯甲醚的转化率达到76.0％,对甲氧基二苯酮(p-MBP)选择性达到97.8％.
参考文献
| [1] | YUAN Bing,QIAO Weihong,LI Zongshi,et al.Application of Zeolite Molecular Sieves in Friedel-Crafts Acylation Reactions[J].Prog Chem,2005,17 (4):686-697 (in Chinese).袁冰,乔卫红,李宗石,等.沸石分子筛在Friedel-Crafts酰基化反应中的应用[J].化学进展,2005,17(4):686-697. |
| [2] | LIU Sen,DU Yunchen,XIAO Ni,et al.One-Pot Synthesis of Mesoporous Fe-SBA-15 and Its Catalytic Performance for Friedel-Crafts Benzylation[J].Chinese J Catal,2008,29 (5):468-472 (in Chinese).刘森,杜耘辰,肖霓,等.一锅法合成介孔材料Fe-SBA-15及其对Friedel-Crafts苄基化反应的催化性能[J].催化学报,2008,29(5):468-472. |
| [3] | Ogoshi S,Nakashima H,Shimonaka K,et al.Novel Role of Carbon Monoxide as a Lewis Acid Catalyst for Friedel-Crafts Reaction[J].J Am Chem Soc,2001,123:8626-8627. |
| [4] | Kawamura M,Cui D M,Hayashi T,et al.Lewis Acid-Catalyzed Friedel-Crafts Acylation Reaction Using Carboxylic Acids as Acylating Agents[J].Tetrahedron Lett,2003,44(42):7715-7717. |
| [5] | Rao L.Solid Acid Catalysts in Green Chemistry[J].Resonance,2007,12(8):30-36. |
| [6] | Sharkawy E A,Shihry S S.Friedel-Crafts Acylation of Toluene Using Superacid Catalysts in a Solvent-Free Medium[J].Monatsh Chem,2010,141:259-267. |
| [7] | Pettinari C.Special Issue:Recent Advances in Organotin Chemistry[J].J Organomet Chem,2006,691:1435-1436. |
| [8] | ZHAO Lifang,WANG Hongshe,MIAO Jianying.Synthesis of Acetals and Ketals Catalyzed by Dibutyltin (Ⅳ) Sulfonates[J].Chinese J Org Chem,2008,28(10):1792-1797(in Chinese).赵立芳,王宏社,苗建英.二丁基锡(Ⅳ)磺酸酯催化合成缩醛(酮)[J].有机化学,2008,28(10):1792-1797. |
| [9] | ZHENG Ying,WANG Xuxu,FU Xianzhi,et al.Surface Organometallic Chemistry:Grafting Reaction of SnMe4 on HY Zeolite Supercage Surface[J].Acta Chim Sin,2004,62 (5):449-453 (in Chinese).郑瑛,王绪绪,付贤智,等.表面金属有机化学:SnMe4在HY沸石超笼表面的接枝反应[J].化学学报,2004,62 (5):449-453. |
| [10] | LIU Xing,SONG Weiming,DENG Qigang.Synthesis of the Trimethyltin Chloride Tethered on Mesoporous Molecular Sieve Al-MCM-41 and Its Catalytic Performance[J].Chinese J Appl Chem,2011,28 (6):673-677 (in Chinese).刘星,宋伟明,邓启刚.介孔分子筛Al-MCM-41接枝三甲基氯化锡的合成、表征及催化性能[J].应用化学,2011,28(6):673-677. |
| [11] | Song W M,Liu X,Jing T,et al.Characterization and Catalytic Properties of Al-MCM-41 Mesoporous Materials by Reactions with Tributyltin Chloride[J].Chinese J Chem Eng,2012,20(5):900-905. |
| [12] | Li Y,Yan B.Photophysical Properties of Lanthanide Hybrids Covalently Bonded to Functionalized SBA-15 by Modified Aromatic Carboxylic Acids[J].J Fluoresc,2009,19:191-201. |
| [13] | Orita A,Otera J.Fluoroalkyldistannoxane Catalysts for Transesterification in Fluorous Biphase Technology[J].Adv Synth Catal,2002,344:84-90. |
| [14] | Grinberg V A,Pasynskii A A,Kulova T L,et al.Tolerant-to-Methanol Cathodic Electrocatalysts Based on Organometallic Clusters[J].Russ J Electrochem,2008,44(2):202-212. |
| [15] | Zhao D Y,Huo Q S,Feng J L,et al.Nonionic Triblock and Star Diblock Copolymer and Oligomeric Surfactant Syntheses of Highly Ordered,Hydrothermally Stable,Mesoporous Silica Structures[J].J Am Chem Soc,1998,120:6024-6036. |
| [16] | Ramaswamy V,Shah P,Lazar K,et al.Synthesis,Characterization and Catalytic Activity of Sn-SBA-15 Mesoporous Molecular Sieves[J].Catal Surv Asia,2008,12:283-309. |
| [17] | Daktemieks D,Baul T S B,Dutta S,et al.Synthesis,Characterization,and X-ray Structures of Diphenyltin(Ⅳ) N-(2-Hydroxyacetophenone) glycinate,Its 1:1 Adduct with Triphenyltin (Ⅳ) Chloride,and Related Systems[J].Organometallics,1998,17:3058-3062. |
| [18] | Orlov A,Zhai Q Z,Klinowski J.Photocatalytic Properties of the SBA-15 Mesoporous Silica Molecular Sieve Modified with Titanium[J].J Mater Sci,2006,41(6):2187-2193. |
| [19] | Chmielarz L,Kus'trowski P,Drozdek M,et al.SBA-15 Mesoporous Silica Modified with Rhodium by MDD Method and Its Catalytic Role for N2O Decomposition Reaction[J].J Porous Mater,2011,18:483-491. |
| [20] | Nguyen L T L,Le K K A,Phan N T S.A Zeolite Imidazolate Framework ZIF-8 Catalyst for Friedel-Crafts Acylation[J].Chinese J Catal,2012,33:688-696. |
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