TETRAHEDRON
LETTERS
Tetrahedron Letters 42 (2001) 4373–4376 Pergamon
Assembling monocyclic, spirocyclic and fused carbocycles by
ring-closing metathesis on an arene–chromium template
Bikash C. Maity, Vishwanath M. Swamy and Amitabha Sarkar*
Divisions of Organic Chemistry (Synthesis), National Chemical Laboratory, Pune 411008, India
Received 26 February 2001; accepted 27 April 2001
Abstract—A variety of diene precursors assembled stereoselectively on an arene–chromium template underwent facile ring-closing
metathesis by ruthenium catalysis at ambient temperature to afford cyclic compounds of varying degrees of complexity in high
yields. © 2001 Elsevier Science Ltd. All rights reserved.
Ring-closing metathesis (RCM) has become a powerful
tool for the ready construction of cyclic structures over
the past few years
1
with the availability of structurally
defined, mononuclear metal catalysts developed by
Schrock
2
[2,6-i Pr
2
C
6
H
3
NMo{OC(CF
3
)
2
Me}
2
CHCMe
2
-
Ph] and Grubbs
3
[Cl
2
{(c -C
6
H
11
)
3
P}
2
RuCHPh]. A sig-
nificant, practical advantage of Grubbs’ ruthenium cat-
alyst is derived from its relative stability to air and
moisture, in addition to its tolerance of a wide variety
of functional groups.
Almost an infinite variety of structures are amenable to
RCM. Since an alkene is the product of metathesis,
chiral cyclic products are usually synthesized from pre-
assembled chiral dienes,
4
while only a few examples
exist in the literature pertaining to chirality originating
from RCM.
5
Arene–chromium complexes provide a ready access to
diastereomerically pure compounds of diverse struc-
tural types.
6
The present report describes the use of
RCM to synthesize a variety of diastereomerically pure
carbocyclic as well as heterocyclic products at ambient
temperature, from differently substituted diene precur-
sors assembled on arene–tricarbonylchromium tem-
plates in high yield. The products are monocyclic,
spirocyclic or fused polycyclic compounds depending
on the design of the precursors, and feature one to
three stereogenic centers. This study complements
recent efforts to create stereochemically defined molecu-
lar scaffolds
7
and the use of organometallic precursors
8
for this purpose.
The substrates were independently synthesized by
appropriate procedures. Complex 1 was synthesized in
three steps from an o -methylacetophenone–Cr(CO)
3
complex. Claisen–Schmidt condensation with p -tolu-
aldehyde was followed by addition of MeLi in ether.
The 1,2-adduct was obtained as the major product
9
and
as a single diastereomer, which was converted to the
allyl ether 1a by a standard procedure. The stereochem-
istry of the new stereogenic center was assigned based
on an exo -selective attack on the sterically preferred
anti conformer.
10
The optically pure substrate 2a was derived from the
optically pure o -anisaldehyde–Cr(CO)
3
complex,
11
the
product resulting from an exo addition to the more
stable anti conformer.
12
The stereochemistry of sub-
strate 3a was assigned on similar considerations. RCM
with Grubbs’ ruthenium catalyst at ambient tempera-
ture in dichloromethane yielded
13
the corresponding
heterocycles in respectable isolated yields (Table 1).
Spirocycles 4b and 5b were similarly obtained from
RCM of relevant substrates 4a and 5a, respectively,
which in turn were prepared by well-precedented
14
exo -
selective allyl Grignard addition to 1-tetralone– and
1-indanone–Cr(CO)
3
complexes.
Based on an earlier report
15
from this laboratory, the
synthesis of substrates 6a and 7a was accomplished
according to the reaction sequence depicted in Scheme
1. * Corresponding author.
0040-4039/01/$ - see front matter © 2001 Elsevier Science Ltd. All rights reserved.
PII:S0040-4039(01)00713-4