Radical cyclization of O-trityl oximino esters: a ring closure that preserves the
oxime function
Derrick L. J. Clive* and Rajendra Subedi
Chemistry Department, University of Alberta, Edmonton, Alberta, Canada T6G 2G2.
E-mail: derrick.clive@ualberta.ca
Received (in Corvallis, OR, USA) 4th November 1999, Accepted 16th December 1999
O-Trityl oximino esters 1 undergo stannane-induced radical
cyclization to regenerate an oxime function, affording
oximino lactones 4; these can be converted into enamides
(e.g. 11b), and such a transformation was used to make the
natural product 14c.
We report radical ring closures of the type summarized in
Scheme 1 (X = homolyzable group).
1,2
The special feature of
such reactions is that the sp
2
status of the acceptor carbon is
preserved—a result that is different from the one seen in the
classical cyclization of hexenyl radicals or the radical cycliza-
tion of O-alkyl oxime ethers.
3–5
Regeneration of the oxime
function after the radical closure must involve
6
tautomerization
of an intermediate nitroso compound, as shown in Scheme 1, 3
? 4.†
The starting oximino esters (cf. 1) are prepared using the
crystalline reagent 5 (mp 165–166 °C), which is easily made
(76%) by stirring equimolar amounts of O-trityl hydroxylamine
and glyoxylic acid monohydrate in THF for 4 h. Evaporation of
Table 1 Esterification of various alcohols and subsequent radical cyclizations
a
Scheme 1
This journal is © The Royal Society of Chemistry 2000
Chem. Commun., 2000, 237–238 237