( ~ ~AHEDRON
LETIERS
Pergamon TetrahedronLetters40 (1999) 8557-8561
Cyclopropane ring formation by an SmI2 mediated cyclisation of
8-halo-ot,13-unsaturated esters
Herv6 David, Carlos Afonso, Martine Bonin, Gilles Doisneau, Made-George Guillerez and
Francois Guib6 *
lnstitut de Chiraie Mol~culaire d'Orsay, Laboratoire de Catalyse Mol~culaire, UPRESA-8075, B,~t. 420, Universitd Paris-Sud,
91405 Orsay, France
Received26 July 1999; accepted21 September1999
Abstract
8-Iodo- and 8-bromo-ct,13-unsaturated esters with various substituents at the 13- and y-positions readily cyclise
to cyclopropane compounds in the presence of samarium diiodide and a proton source. © 1999 Elsevier Science
Ltd. All rights reserved.
Keywords: samarium;samariumcompounds;radical reactions;cyclisations; cyclopropanes.
Since the seminal report by Kagan and co-workers, ! SmI2 has found many applications in synthetic
organic chemistry. In particular, SmIE-mediated sequenced radical-anionic or anionic-radical reactions
are of great interest for the synthesis of various carbocyclic and heterocyclic molecules, as amply
demonstrated especially by Molander and co-workers. 2 Up to now, these reactions have been essentially
used for the obtention of five- or six-membered rings. For instance, Molander and Harris recently
described the SmI2-induced cyclisation of ~- and q-iodo-et,13-unsaturated esters to 1-carbalkoxyalkyl-
substituted cyclopentane or cyclohexane derivatives. 3 In the present communication, we report that 8-
iodo- and 8-bromo-ot,[~-unsaturated esters also cyclise in the presence of SmI2, leading to cyclopropane
compounds. 4
O2Bn O2Bn
a:X=l
1 b:X= Br 2 3 4
c:X=H
In a first experiment, we found that benzyl 5-iodopent-2-enoate la reacted with SmI2 (2.5 equiv, as a
0.1 M solution in THF) in the presence of HMPA (4 equiv.) within 5 min at room temperature to give,
* Corresponding author.Tel: +33-01-69-15-52-59; fax: +33-01-69-15-46-80; e-maih fraguibe@icmo.u-psud.fr
0040-4039/99/5 - see frontmatter © 1999 Elsevier Science Ltd. All rightsreserved.
PII: S0040-4039(99)01816-X