[1]方永勤,王兆岗,吕新宇.对氟甲苯液相氧化制备对氟苯甲醛[J].常州大学学报(自然科学版),2011,(02):32-35.
 FANG Yong-qin,WANG Zhao-gang,LV Xin-yu.Study of the Synthesis of p-Fluorobenzaldyhyde by Oxidizing p-Fluorotoluene in Liquid Phase[J].Journal of Changzhou University(Natural Science Edition),2011,(02):32-35.
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对氟甲苯液相氧化制备对氟苯甲醛()
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常州大学学报(自然科学版)[ISSN:2095-0411/CN:32-1822/N]

卷:
期数:
2011年02期
页码:
32-35
栏目:
出版日期:
2011-03-30

文章信息/Info

Title:
Study of the Synthesis of p-Fluorobenzaldyhyde by Oxidizing p-Fluorotoluene in Liquid Phase
作者:
方永勤王兆岗吕新宇
常州大学 设计研究院,江苏 常州 213164
Author(s):
FANG Yong-qinWANG Zhao-gangLV Xin-yu
Institute of Design and Research,Changzhou University,Changzhou 213164,China
关键词:
对氟甲苯 对氟苯甲醛 对氟苯甲酸 液相氧化
Keywords:
p-fluorotoluene p-fluorobenzaldehyde p-fluorobenzoic acid liquid phase oxidation
分类号:
TQ 245.3
文献标志码:
A
摘要:
以对氟甲苯为原料,Co/Mn/Br为催化体系,氧气为氧化剂,常压下液相氧化制备对氟苯甲醛,探讨了催化剂配比、催化剂用量、反应温度、溶剂用量、氧气流量对氧化反应的影响。较优工艺条件为:90 ℃,氧气12.5 mL/min,n(Co):n(Mn):n(Br)=1:2:1.5,催化剂用量2.0%(以对氟甲苯计),m(乙酸):m(对氟甲苯)=4:1,反应8 h,对氟甲苯转化率35.3%,对氟苯甲醛选择性57.4%。
Abstract:
p-Fluorobenzaldehyde was prepared by oxidizing p-fluorotoluene in Co/Mn/Br catalytic system, using oxygen as oxidant under atmospheric condition. The influence of catalyst ratio and dosage, temperature, solvent amount, oxygen flow on the oxidation reaction were investigated. The optimalconditions were as follow: reaction at 90 ℃, oxygen flow 12.5 mL/min, n(Co):n(Mn):n(Br)=1:2:1.5, adding dosage was 2.0%(counted with the mass of p-fluorotoluene),m(acetic acid):m(p-fluorotoluene)=4:1, reaction time was 8h, the conversion of p-fluorotoluene was 35.3%, the selectivity of p-fluorobenzaldehyde was 57.4%.

参考文献/References:

[1]William S R,Timothy N S,Zhao L S,et al.Process for Preparing Intermediates for the Synthesis of Paroxetine:WO,2009005647[P].2009-01-08.
[2]黄仲斌,戴连华,谌谆,等.一种用于合成瑞舒伐他汀中间体及瑞舒伐他汀的合成方法:中国,101376647[P].2009-03-04.
[3]颜汉新.一种用对氟苯甲醛合成氟氯氰菊酯的方法:中国,1508124[P].2004-06-30.
[4]Toshiya M,Shiro K,Hiroshi H,et al.Synthesis and biological activities of the optical isomers of(±)-4-amino-5-chloro-2-ethoxy-N-[
[4-(4-fluorobenzyl)-2-morpholinyl]methyl]benzamide(mosapride)[J].Chem Pharm Bull,1994,42(4):82-87.
[5] 梁政勇,吕春绪,李斌栋.微波作用下卤素交换氟化制备氟代苯甲醛及二苯甲酮类化合物[J].化学通报,2006,11:836-841.
[6]刘宇.对氟苯甲醛的合成[J].精细化工,2003,20(8):506-508.
[7]Glbert B,Peter B.Process for Prepearing Aromatic Aldehyde:US,5347054[P].1994-09-13.
[8]盛梅,肖建东,林西平,等.甲苯在V2O5/α-Al2O3催化剂上的选择性氧化V2O5负载量对催化剂性能的影响[J].精细石油化工,1999(1):21-25.
[9]Groves J T,Nemo T E,Myers R S.Hydroxylation and epoxidation catalyzed byiron-porphine complexes.Oxygen transfer from iodosylbenzene[J].J Am Chem Soc,1979,101(4):1 032-1 033.
[10]Hu A J,Wang H Y,Li B D.Selective oxidation of p-chlorotoluene with Co(OAc)2/MnSO4/KBr in acetic acid-water medium[J].Catal Commun,2007,8:1 279-1 283.
[11]成有为,王丽军,谢刚,等.MC(Mid-Century)催化氧化过程的研究进展[J].化工进展,2005,24(8):837-840.
[12]杨学萍.对二甲苯氧化制备对苯二甲酸催化体系的研究进展[J].工业催化,2004,12(6):25-29.
[13]谢刚,成有为,李希.对二甲苯液相氧化催化机理[J].聚酯工业,2002,15(4):1-4.
[14]Partenheimer W.The structure of metal/bromide catalysts in acetic acid/water mixtures and its significance in autoxidation[J].J Mol Catal A:Chem,2001,174:29-33.
[15]Partenheimer W.Methodology and scope of metal/bromide autoxidation of hydrocarbons[J].Catal Today,1995,23:69-158.

相似文献/References:

[1]方永勤,席化远.对氟苯甲酰氯的合成[J].常州大学学报(自然科学版),2012,(01):18.
 FANG Yong-qin,XI Hua-yuan.Synthesis of p-Fluorobenzoyl Chloride[J].Journal of Changzhou University(Natural Science Edition),2012,(02):18.

备注/Memo

备注/Memo:
作者简介:方永勤(1966-),女,江苏姜堰人,研究员级高级工程师。
更新日期/Last Update: 2011-03-30