TETRAHEDRON
LETTERS
Tetrahedron Letters 43 (2002) 7201–7203 Pergamon
Solid phase-mediated synthesis of isonitriles
Delphine Launay,
a
Susan Booth,
b
Ian Clemens,
c
Andrew Merritt
d
and Mark Bradley
a,
*
a
Combinatorial Centre of Excellence, Department of Chemistry, University of Southampton, Southampton SO17 1BJ, UK
b
Organon, Newhouse, Lanarkshire, Scotland, UK
c
Eli Lilly & Co., Lilly Research Centre, Erl Wood Manor, Windlesham, Surrey GU20 6PH, UK
d
GSK, Research and Development, Medicines Research Centre, Gunnels Wood Road, Stevenage SG12NY, UK
Received 12 February 2002; revised 2 August 2002; accepted 9 August 2002
Abstract—Supported sulfonyl chlorides and microwave irradiation are an efficient combination for isonitrile synthesis. © 2002
Elsevier Science Ltd. All rights reserved.
Multi-component reactions (MCRs) have become an
important constituent of the combinatorial chemist’s
arsenal, allowing large numbers of compounds to be
produced in a rapid parallel synthesis programme.
Thus, the Passerini
1
and Ugi
2
reactions, to name but
two, have become well established in library synthesis
programmes (Scheme 1).
3
One of the most important components of these reac-
tions, and one that is very limited in accessibility, is the
isonitrile. Isonitriles are especially important due to
their unusual bifunctional reactivity, acting as both a
nucleophile and an electrophile during the reaction.
There are numerous methods reported for isonitrile
synthesis,
4
however, during the synthesis of a series of
isonitrile tags we became aware of the limited utility
and applicability of many current methods. Eventually
the synthetically most useful conditions, the treatment
of formamides with p -toluene sulfonyl chloride, were
identified
5
and this led to the synthesis of a number of
isonitriles in reasonable yield and purity (Scheme 2).
Scheme 2. Solution synthesis of isonitiriles.
Work-up and purification of this reaction was problem-
atic due to the reactivity of the isonitriles. The use of a
polymer supported sulfonyl chloride therefore appeared
to offer a fast and efficient method of isonitrile genera-
tion, with just a simple filtration and acidic work-up (to
remove the pyridine) being involved. A number of
reactions were therefore investigated using a range of
formamides, as shown in Table 1 and Scheme 3.
Scheme 1. (a) Passerini and (b) Ugi reaction.
* Corresponding author.
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