以乙二胺四乙酸二钠(EDTA)、柠檬酸、草酸、酒石酸改性制备了H-BEA,并根据XRD和NH3-TPD对沸石H-BEA进行表征.采用上述改性沸石催化4-苯基丁酸分子内付克反应合成1-萘满酮进行催化剂反应活性评价.实验结果表明,以柠檬酸改性沸石H-BEA具有较高的催化活性.进一步对催化剂用量、反应温度、反应时间等工艺条件优化得到最佳工艺条件,在最佳工艺条件下,产物1-萘满酮产率达到94.3%.
Zeolite H-BEA modified by ethylene diamine tetraacetic acid(EDTA),citric acid,oxalic acid,and tartaric acid were prepared and characterized by XRD and NH3-TPD.The catalytic performance was evaluated in the synthesis of 1-tetralone by intramolecular Friedel-Crafts reaction of 4-phenylbutyric acids.Zeolites H-BEA modified by citric acid showed high catalytic activity.In addition,the reaction conditions such as catalyst amount,reaction temperature and reaction time were examined for the optimal process conditions.Under the optimal reaction conditions,the yield for 1-tetralone was 94.3%.
参考文献
[1] | Shimada S,Sai T.Method for Manufacturing Chromanones or Thiochromanones.Japan 189695[P],2004. |
[2] | Shimada S,Sai T.Method for Producing Cylic Ketones.Japan 189620[P],2004. |
[3] | Cui D M,Kawamura M,Shimada S,et al.Synthesis of 1-Ttetralones by Intramolecular Friedel-Crafts Reaction of 4-Arylbutyric Acids Using Lewis Acid Catalysts[J].Tetrahedron Lett,2003,44:4007-4010. |
[4] | Cui D M,Zhang C,Kawamura M,et al.Synthesis of 1-Indanones by Intramolecular Friedel-Crafts Reaction of 3-Arylpropionic Acids Catalyzed by Tb(OTf)3[J].Tetrahedron Lett,2004,45:1741-1745. |
[5] | WU Zhengduo,HUANG Ddongmei.Synthesis of α-Tetralone[J].Liaoning Chem Ind,2001,30(2):83-83,92(in Chinese).吴正铎,黄冬梅.α-萘满酮的合成[J].辽宁化工,2001,30(2):83-83,92. |
[6] | Hiroki K,Hatori M,Yamashita H,et al.Efficient Synthesis of 1-Tetralones from 4-Arylnutyric Acids by Combined Use of Solid Acid Catalysts and Microwave Irradiation[J].Chem Lett,2008,37(3):320-321. |
[7] | WU Guang,ZHOU Dapeng,HAN Xue,et al.Study on Surface Acidity of Modified HY Zeolite by NH3-TPD Method[J].Chem Adhes,2006,28(1):17-19(in Chinese).武光,周大鹏,韩雪,等.用NH3-TPD研究改性HY沸石的表面酸性[J].化学与粘合,2006,28(1):17-19. |
- 下载量()
- 访问量()
- 您的评分:
-
10%
-
20%
-
30%
-
40%
-
50%