Pergamon
Tetrahedron Letters 40 (1999) 1627-1630
TETRAHEDRON
LETTERS
Highly Effective Synthesis of 4-1talo-Tetrahydropyrans Via A Highly
Diastereoselective in situ Prins-Type Cyclization Reaction
Jun Yang, Ganapathy S. Viswanathan and Chao-Jun Li*
Department of Chemistry
Tulane University
New Orleans, Louisiana 70118, USA
Received 10 November 1998; accepted 22 December 1998
Abstract: The reaction of aldehyde with homoaUylalcohols mediated by indium trichloride generated
4-chlorotetrahydropyrans in high yields and with high stereoselectivity. The same type of compounds
can be generated through a single step, multi-component coupling between aldehyde and allyl bromide
mediated by indium O 1999ElsevierScienceLtd. All rightsreserved.
The acid-catalyzed olefin-aldehyde condensation, known as the Prins reaction, is a fundamental
reaction for carbon-carbon bond formation.1 However, the synthetic application of this important reaction has
been underexplored due to the classical conditions of strong acids (e.g., sulfuric acid) and high reaction
temperatures, which often generated a range of products. The pyran ring is part of the backbone of various
important carbohydrates and natural products. 2 Recently, during our investigation of indium-mediated
reactions under neat conditions (Eq. 1),3 we sometimes observed an instant polymerization of the reaction
mixture. Although they initially eluded our attention, a subsequent analysis of the mixture revealed the
presence of small amount of tetrahydropyran derivatives.4
Br OH
o ,n
2 .~ + ~Br " + (1)
R H R R R R
R= Ph- 54% 25%
R= MePh-24% 17%
To explain the formation of the tetrahydropyran derivatives, we postulated that the product was
generated through a tandem carbonyl allylation-hemiacetal formation-Prins reaction (Scheme 1). In order to
test the viability of the proposed reaction pathway, we conceived that the reaction of a homoallyl alcohol with
an aldehyde should generate the corresponding tetrahydropyran derivatives in the presence of an indium halide.
In addition, the reaction could be pushed to a single 4-halo derivative rather than a mixture of alcohol and
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