Synthesis of methyl acetoacetate from acetone and dimethyl carbonate with alkali-promoted MgO catalysts

被引:7
作者
Wu, Dudu [1 ]
Chen, Zhi [1 ]
机构
[1] Guangdong Med Coll, Sch Pharm, Dongguan 523808, Peoples R China
来源
CHEMICAL PAPERS | 2010年 / 64卷 / 06期
关键词
methyl acetoacetate; acetone; dimethyl carbonate; MgO; alkali metals; PHASE-TRANSFER CATALYSIS; ALDOL CONDENSATION; DIALKYL CARBONATES; O-METHYLATION; CATECHOL;
D O I
10.2478/s11696-010-0068-9
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
The synthesis of methyl acetoacetate (MAA) by methoxycarbonylation of acetone with dimethyl carbonate (DMC) was carried out in the presence of MgO and alkali-promoted MgO catalysts. From among Li, Na, K, and Cs, potassium was found to be the most effective promoter to improve the activity of MgO. The effect of K/MgO with variable content of K was also investigated, and the individual catalysts were characterised by the XRD, BET, SEM, CO2-TPD, and in situ CO2 IR techniques. The results showed that the addition of a small amount of K (1.97 mass %) could promote MAA formation, but a higher K loading caused a decrease in the yield of MAA, which might result from particle agglomeration and the presence of stable potassium carbonates. In situ FTIR experiments of co-adsorbed reactants indicated that the reaction probably proceeded via abstraction of H-alpha from acetone by base sites. (C) 2010 Institute of Chemistry, Slovak Academy of Sciences
引用
收藏
页码:758 / 766
页数:9
相关论文
共 25 条
[1]   Spectroscopic and kinetic study of the alkylation of phenol with dimethyl carbonate over NaX zeolite [J].
Beutel, T .
JOURNAL OF THE CHEMICAL SOCIETY-FARADAY TRANSACTIONS, 1998, 94 (07) :985-993
[2]   Base catalysis for the synthesis of alpha,beta-unsaturated ketones from the vapor-phase aldol condensation of acetone [J].
DiCosimo, JI ;
Diez, VK ;
Apesteguia, CR .
APPLIED CATALYSIS A-GENERAL, 1996, 137 (01) :149-166
[3]   Aldol condensation of citral with acetone on MgO and alkali-promoted MgO catalysts [J].
Diez, V. K. ;
Apesteguia, C. R. ;
Di Cosimo, J. I. .
JOURNAL OF CATALYSIS, 2006, 240 (02) :235-244
[4]   Acid-base properties and active site requirements for elimination reactions on alkali-promoted MgO catalysts [J].
Díez, VK ;
Apesteguía, CR ;
Di Cosimo, JI .
CATALYSIS TODAY, 2000, 63 (01) :53-62
[5]  
Fischer R., 1995, Patent, Patent No. [US5453535, 5453535]
[6]   Vapor-phase reactions of catechol with dimethyl carbonate. Part I. O-methylation of catechol over alumina [J].
Fu, Y ;
Baba, T ;
Ono, Y .
APPLIED CATALYSIS A-GENERAL, 1998, 166 (02) :419-424
[7]   Selective O-methylation of catechol using dimethyl carbonate over calcined Mg-Al hydrotalcites [J].
Jyothi, TM ;
Raja, T ;
Talawar, MB ;
Rao, BS .
APPLIED CATALYSIS A-GENERAL, 2001, 211 (01) :41-46
[8]  
KANNO T, 1994, STUD SURF SCI CATAL, V90, P207
[9]  
KOEHLER G, 1998, Patent No. 5786502
[10]  
Koehler G., 1995, Patent, Patent No. [US5436365, 5436365]