Using in situ Raman monitoring as a tool for rapid optimisation and scale-up of microwave-promoted organic synthesis:: esterification as an example

被引:25
作者
Leadbeater, Nicholas E.
Smith, Rebecca J.
Barnard, T. Michael
机构
[1] Univ Connecticut, Dept Chem, Storrs, CT 06269 USA
[2] CEM Microwave Technol, Matthews, NC 28106 USA
关键词
D O I
10.1039/b615597a
中图分类号
O62 [有机化学];
学科分类号
070303 ; 081704 ;
摘要
Microwave-promoted esterification reactions have been monitored using in situ Raman spectroscopy. Having optimised a reaction on a 23 mmol scale, it was transferred to a larger reaction vessel and scaled up to 0.26 mol, again with Raman monitoring. With conditions in hand, an automated stop-flow apparatus was used to prepare 5.7 moles of product.
引用
收藏
页码:822 / 825
页数:4
相关论文
共 34 条
[11]   Enzymatic esterification between n-alcohol homologs and n-caprylic acid in non-aqueous medium under microwave irradiation [J].
Huang, W ;
Xia, YM ;
Gao, H ;
Fang, YJ ;
Wang, Y ;
Fang, Y .
JOURNAL OF MOLECULAR CATALYSIS B-ENZYMATIC, 2005, 35 (4-6) :113-116
[12]   Controlled microwave heating in modern organic synthesis [J].
Kappe, CO .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2004, 43 (46) :6250-6284
[13]  
Kappe CO, 2005, METH PRIN MED CHEM, V52, P1, DOI 10.1002/3527606556
[14]   Microwave-accelerated homogeneous catalysis in organic chemistry [J].
Larhed, M ;
Moberg, C ;
Hallberg, A .
ACCOUNTS OF CHEMICAL RESEARCH, 2002, 35 (09) :717-727
[15]   Real-time monitoring of microwave-promoted Suzuki coupling reactions using in situ Raman spectroscopy [J].
Leadbeater, Nicholas E. ;
Smith, Rebecca J. .
ORGANIC LETTERS, 2006, 8 (20) :4588-4591
[16]   Increasing rates of reaction: Microwave-assisted organic synthesis for combinatorial chemistry [J].
Lew, A ;
Krutzik, PO ;
Hart, ME ;
Chamberlin, AR .
JOURNAL OF COMBINATORIAL CHEMISTRY, 2002, 4 (02) :95-105
[17]   Microwave assisted organic synthesis -: a review [J].
Lidström, P ;
Tierney, J ;
Wathey, B ;
Westman, J .
TETRAHEDRON, 2001, 57 (45) :9225-9283
[18]  
Lidstrom P., 2005, MICROWAVE ASSISTED O
[19]  
Loupy A., 2006, MICROWAVES ORGANIC S, DOI DOI 10.1002/9783527619559
[20]  
Loupy A., 2002, MICROWAVES ORGANIC S