高效液相色谱法测定固体酸催化1,4-二甲氧基苯乙酰化反应产物
HPLC Determination Reaction Product of Solid Acid-Catalytic Acetylation of 1,4-Dimethoxybenzene
摘 要
提出了高效液相色谱法测定固体酸催化1,4-二甲氧基苯乙酰化反应产物2,5-二甲氧基苯乙酮的方法.高效液相色谱柱为ODS-C18反相柱(250 mm×4.6 mm,5 μm),甲醇-水(80+20)溶液为流动相,检测波长为250 nm.在此检测条件下,2,5-二甲氧基苯乙酮检测量在 0.277~2.777 mmol·L-1范围与其峰面积呈线性关系.该方法可迅速准确地用于固体酸催化的1,4-二甲氧基苯乙酰化反应转化率的测定.
2,5-二甲氧基苯乙酮
1,4-二甲氧基苯
乙酰化
固体酸
HPLC
2,5-Dimethoxyacetophenone
1,4-Dimethoxybenzene
Acetylation
Solid acid
Abstract
HPLC was applied to determination of reaction product,namely 2,5-dimethoxyacetophenone,of the solid acid catalytic acetylation of 1,4-dimethoxybenzene.ODS-C18 RP column (250 mm×4.6 mm,5 μm) was used as stationary phase,and ethanol-H2O (80+20) solution was used as mobile phase.UV-detection at the wavelength of 250 nm was adopted in the measurement.Under the prescribed conditions,linearity range of 0.277-2.777 mmol·L-1 of 2,5-dimethoxyacetophenone was found with the values of peak areas.The proposed method was used to monitor and control the conversion rate of the acetylation of 1,4-dimethoxybenzene.
中图分类号 O657.7
所属栏目 试验与研究
基金项目 国家自然科学基金项目(20776035);河北省首批百名创新人才基金项目
收稿日期 2008/2/19
修改稿日期
网络出版日期
作者单位点击查看
备注冯磊(1982-),男,河北石家庄人,硕士生,研究方向为固体酸催化.
引用该论文: FENG Lei,ZHANG Yue-cheng,GUO Feng,ZHAO Ji-quan,ZHANG Song-mei. HPLC Determination Reaction Product of Solid Acid-Catalytic Acetylation of 1,4-Dimethoxybenzene[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(10): 921～923
冯磊,张月成,郭峰,赵继全,张松梅. 高效液相色谱法测定固体酸催化1,4-二甲氧基苯乙酰化反应产物[J]. 理化检验－化学分册, 2008, 44(10): 921～923
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】Giordano C,Villa M,Annunziata R.Mild and reversible friedel-crafts acylation: synthesis of 6-acyl-2-methoxynaphthalene[J].Syn Comm,1990,20(3):383-392．
【2】陈冠凡,林原斌,黄红霞.2,5-二甲氧基乙苯的合成方法及改进[J].合成化学,2003,11(5):443-444．
【3】Ameer F,Gilles R G F,Green I R,et al.Synthesis of methoxy-2-hydroxy-1,4-naphthoquinones and reaction of one isomer with aldehydes under basic conditions[J].Syn Comm,2004,34(7):1247-1258．
【4】Yadav G D,Pimparkar K P.Insight into Friedel-Crafts acylation of 1,4-dimethoxybenzene to 2,5-dimethoxyacetophenone catalysed by solid acids-mechanism,kinetics and remedies for deactivation[J].J Mol Catal A: Chem,2007,264:179-191．
【5】Breda A,Signoretto M,Ghedini E,et al.Acylation of veratrole over promoted SZ/MCM-41 catalysts: Influence of metal promotion[J].Appl Catal A,2006,308:216-222．
【6】Alizadeh A,Khodaei M M,Nazari E.Notes silica sulfuric acid as an efficient solid acid catalyst for friedel-crafts acylation using anhydrides[J].Bull Korean Chem Soc,2007,28(10):1854-1856．
【7】Selvaraj M,Pandurangan A,Seshadri K S,et al.Synthesis of ethyl β-naphthyl ether(neroline)using SO2-4/Al-MCM-41 mesoporous molecular sieves[J].J Mol Catal A: Chem,2003,192:153-170．
【8】Sinnerma A,Jansen R J J,Pamin K,et al.New acid catalyst comprising heteropoly acid on a mesporous sieve MCM-41[J].Catal Lett,1995,30:241-250．
【9】Grun M,Unger K K,Matsumoto A,et al.Novel pathways for the preparation of mesoporous MCM-41 materials:control of porosity and morphology[J].Microporous Mesoporous Mater,1999,27:207-216．
【10】邹凌峰.NaY晶化母液制备硅铝胶的技术探讨[J].工业催化,2002,10(6):56-60．
【2】陈冠凡,林原斌,黄红霞.2,5-二甲氧基乙苯的合成方法及改进[J].合成化学,2003,11(5):443-444．
【3】Ameer F,Gilles R G F,Green I R,et al.Synthesis of methoxy-2-hydroxy-1,4-naphthoquinones and reaction of one isomer with aldehydes under basic conditions[J].Syn Comm,2004,34(7):1247-1258．
【4】Yadav G D,Pimparkar K P.Insight into Friedel-Crafts acylation of 1,4-dimethoxybenzene to 2,5-dimethoxyacetophenone catalysed by solid acids-mechanism,kinetics and remedies for deactivation[J].J Mol Catal A: Chem,2007,264:179-191．
【5】Breda A,Signoretto M,Ghedini E,et al.Acylation of veratrole over promoted SZ/MCM-41 catalysts: Influence of metal promotion[J].Appl Catal A,2006,308:216-222．
【6】Alizadeh A,Khodaei M M,Nazari E.Notes silica sulfuric acid as an efficient solid acid catalyst for friedel-crafts acylation using anhydrides[J].Bull Korean Chem Soc,2007,28(10):1854-1856．
【7】Selvaraj M,Pandurangan A,Seshadri K S,et al.Synthesis of ethyl β-naphthyl ether(neroline)using SO2-4/Al-MCM-41 mesoporous molecular sieves[J].J Mol Catal A: Chem,2003,192:153-170．
【8】Sinnerma A,Jansen R J J,Pamin K,et al.New acid catalyst comprising heteropoly acid on a mesporous sieve MCM-41[J].Catal Lett,1995,30:241-250．
【9】Grun M,Unger K K,Matsumoto A,et al.Novel pathways for the preparation of mesoporous MCM-41 materials:control of porosity and morphology[J].Microporous Mesoporous Mater,1999,27:207-216．
【10】邹凌峰.NaY晶化母液制备硅铝胶的技术探讨[J].工业催化,2002,10(6):56-60．
相关信息
