Pergamon
Tetrahedron Letters, Vol. 38, No. 10, pp. 181%1820, 1997
O 1997 Elsevier Science lad
All rights reserved.Printed in Great Britain.
PII: S0040-4039(97)00159-7 0040-4039/97 $17.00 + 0.00
Chemoselective Addition of Grignard Reagents to Aikoxycarbonylalkyl-
N-imidazolium-N-methyl Amides: Synthesis of 4-Oxo and Homologous Esters
Maria A. de las Heras, Juan J. Vaquero, Jos~ L. Garcia-Navio, Julio Alvarez-Builla*
Departamento de QuimicaOrganica, Universidadde Alcalfi, 2887 l-Alcal~i de Henares, Madrid. Spain.
Abstract: A method for the synthesis of 4-oxo and homologous esters is achieved by metalation of
alkoxycarbonylalkyl-N-imidazolium-N-methyl amideswith Iequiv of LDA followed by highlyehemoseleetive
addition of 1 equiv ofa Grignard reagent. © 1997 Elsevier Science Ltd. All fights reserved.
Although it has been known for a long time that the carbonyi group can be formed by reacting organometallics
with carboxylic acid derivatives,1 only with the development of selective acylating reagents 2 (e.g. Weinreb's
amide 3'4) has this reaction proved to be of synthetic utility. Recently, we demonstrated that N-imidazolium-N-
methylamides I and bis-amides 2 behave as highly selective acylating reagents towards organometallics leading in
good to excellent yields to ketones 5 and diketones. Moreover, the 1-(N-alkoxyoxalyl-N-methylamino)-3-
methylimidazolium salts 3 were shown to yield 2-oxo esters by addition of Grignard reagents 7 whereas in the case
of the equivalent Weinreb type amide 4 the addition of an aliphatic organometallic takes place on the ester group
leading to undesired 2-oxo amides 8 (Scheme 1).
Me,,
N O
/'~ + "
~.,- N .. N ..JL. R
_ o
× , N EIF
Me R... OEt R1-M
Me 1 Me Me O
/
"~N'N" "y" "N "N'~ R 1= Aliphatic
X- Me IVle X- a=Li, agX
Me
o
3R= ~N*= R'%OEt
O
4: R = OMe
O
R--.N%RI
Me O
Scheme 1
1817