欢迎登录材料期刊网

材料期刊网

高级检索

采用硅胶负载Keggin型H6PM09V3O40催化水杨醛与硝酸反应合成5-硝基水杨醛,考察了催化剂负载量、反应时间、反应温度、催化剂用量、硝酸用量和溶剂对反应的影响及催化剂的重复使用性能.实验结果表明,m(水杨醛)∶m(质量分数65%硝酸)∶m(负载量20% H6 PM09 V3 O40/SiO2)=2.44∶3.00∶3.00,用石油醚作为溶剂,45℃反应2.5h,水杨醛的转化率为98%,5-硝基水杨醛的选择性为96.8%.催化剂回收容易,重复使用5次后,活性基本不变.

参考文献

[1] Tomoyo S,Yan Y L,Marriott G,et al.Family of Site-Selective Molecular Optical Switches[J].J Org Chem,2005,70 (6):2009-2013.
[2] Zhu L Y,Khairttdinov B F,Cape J L,et al.Photoregulated Transmembrane Charge Separation by Linked Spiropyran-Anthraquinone Molecules[J].JAm Chem Soc,2006,128(3):825-835.
[3] Yildiz I,Impellizzeri S,Deniz E,et al.Supramolecular Strategies to Construct Biocompatible and Photoswitchable Fluorescent Assemblies[J].J Am Chem Soc,2011,133(4):871-879.
[4] LIU Cuiying,LI Zhong,LIU Peiman,et al.Synthesis and Antibacterial Activities of 5-Nitro-N-(2-hydroxyethyl)salicylaldimine with Copper(Ⅱ)[J].West China J Pharm Sci,1996,11 (2):69-71 (in Chinese).柳翠英,李忠,刘培漫,等.5-硝基水杨醛亚胺合铜(Ⅱ)类螯合物的合成与抑菌活性[J].华西药学杂志,1996,11(2):69-71.
[5] Yildiz M,Dulger B,Koyuncu S Y,et al.Synthesis and Antimicrobial Activity of Bis (imido) Schiff Bases Derived from Thiosemicarbazide with Some 2-Hydroxyaldehydes and Metal Complexes[J].J Indian Chem Soc,2004,81 (1):7-12.
[6] Mustafa I M,Hapipah M A,Abdulla M A,et al.Synthesis,Structural Characterization,and Anti-ulcerogenic Activity of Schiff Base Ligands Derived fron Tryptamine and 5-Chloro,5-Nitro,3,5-Ditertiarybutyl Salicylaldehyde and Their Nickel (Ⅱ),Copper(Ⅱ),and Zinc(Ⅱ) Complexes[J].Polyhedron,2009,28(18):3993-3998.
[7] Gottker-Schnetmann I,Wehrmann P,Rohr C,et al.Substituent Effects in (k2-N,O)-Salicylaldiminato Nickel (Ⅱ)-Methyl Pyridine Polymerization Catalysts:Terphenyls Controlling Polyethylene M icrostructures[J].Organometallics,2007,26 (9):2348-2362.
[8] Chen L J,Bao J,Mei F M,et al.Oxidative Carbonylation of Aniline to N,N'-Diphenyl Urea Catalyzed by Cobalt (Ⅱ)-Schiff Base Complex/Pyridine Catalytic System[J].Catal Commun,2008,9(5):658-663.
[9] Hashimoto J,Motohashi K,Sakamoto K,et al.Screening and Evaluation of New Inhibitors of Hepatic Glucose Production[J].J Antibiotics,2009,62 (11):625-629.
[10] BU Xinyu,ZHANG Hua,LI Yaming,et al.Reviews on Synthetic Methods of 5-Nitrosalicylaldehyde[J].Fine Chem Intermed,2004,35(3):4-6 (in Chinese).卜鑫宇,张华,李亚明,等.5-硝基水杨醛合成方法[J].精细化工中间体,2004,35(3):4-6.
[11] ZHANG Weiqing,WANG Jingbing,ZHOU Shibiao,et al.The Reform of 5-Nitrosalcylaldehyde Nitrifying Means[J].J Hunan Univ Arts Sci(Nat Sci Edn),2006,18(1):31-33(in Chinese).张维庆,王景炳,周诗彪,等.5-硝基水杨醛硝化法的改进[J].湖南文理学院学报(自然科学版),2006,18(1):31-33.
[12] Bose A K,Ganguly S N,Manhas M S,et al.Microwave Promoted Rapid Nitration of Phenolic Compounds with Calcium Nitrate[J].Tetrahedron Lett,2006,47(12):1885-1888.
[13] Selvam J J P,Suresh V,Rajesh K,et al.Highly Efficient Nitration of Phenolic Compounds by Zirconyl Nitrate[J].Tetrahedron Lett,2006,47(15):2507-2509.
[14] Heravi M M,Benmorad T,Bakhtiari K,et al.H3+x PMo12-x VxO40 (Heteropolyacids)-Catalyzed Regioselective Nitration of Phenol to o-Nitrophenol in Heterogeneous System[J].J Mol Catal A:Chem,2007,264(1/2):318-321.
[15] QIAN Hua,LIU Dabin,YE Zhiwen.Selective Nitration of Chlorobenzene with N2O5 Assisted by Supported Heteropoly Acids[J].Chinese J Appl Chem,2009,26(6):676-680(in Chinese).钱华,刘大斌,叶志文.负载杂多酸催化下N2O5对氯苯的选择性硝化[J].应用化学,2009,26(6):676-680.
[16] ZHANG Jin,TANG Ying,LUO Qian,et al.Study on the Synthesis of Heteropoly Acids Containing Different Amount of V and Mo and Their Catalytic Performance for the Direct Hydroxylation of Benzene to Phenol[J]. Chinese J Inorg Chem,2004,20(8):935-940 (in Chinese).张进,唐英,罗茜,等.钼钒磷杂多酸的合成及催化性能研究[J].无机化学学报,2004,20(8):935-940.
[17] GONG Shuwen,WANG Xiangyu,LIU Lijun,et al. Nitration of Benzene Catalyzed by Supported Ammonium Phosphotungstate Catalyst[J].Chem Reag,2010,32 (4):341-344 (in Chinese).龚树文,王向宇,刘丽君,等.负载磷钨酸铵催化苯硝化反应的研究[J].化学试剂,2010,32(4):341-344.
[18] CHENG Guangbin.Study on Regioselective Nitration of Aromatic Compounds on Solid Acid Catalysts[D].Nanjing:Nanjing University of Science and Technology,2002(in Chinese).程广斌.固体催化剂上芳香族化合物区域选择性硝化反应研究[D].南京:南京理工大学,2002.
[19] Dagade S P,Kadam V S,Dongare M K.Regioselective Nitration of Phenol over Solid Acid Catalysts[J].Catal Commun,2002,3(2):67-70.
[20] HE Yigong,LI Fen,WANG Peng,et al.Adsorption,Acidity and Physico-Chemical Properties of Heteropoly Acid Catalysts[J].Pet Process Petrochem,1996,27 (8):12-16(in Chinese).何奕工,李奋,王蓬,等.杂多酸催化剂的吸附、酸性和物化性质[J].石油炼制与化工,1996,27(8):12-16.
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:
  • 1
    0%
  • 2
    0%
  • 3
    0%
  • 4
    0%
  • 5
    0%