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  4. Competition between hetero-Diels-Alder and cheletropic addition of sulfur dioxide. Theoretical and experimental substituent effects on the relative stability of 3,6-dihydro-1,2-oxathiin-2-oxides (sultines) and 2,5-dihydrothiophene-1,1-dioxides (sulfolenes). Anomeric effects in sultine and 6-substituted derivatives
 
research article

Competition between hetero-Diels-Alder and cheletropic addition of sulfur dioxide. Theoretical and experimental substituent effects on the relative stability of 3,6-dihydro-1,2-oxathiin-2-oxides (sultines) and 2,5-dihydrothiophene-1,1-dioxides (sulfolenes). Anomeric effects in sultine and 6-substituted derivatives

Fernandez, T.
•
Suarez, D.
•
Sordo, J. A.
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1998
The Journal of Organic Chemistry

At low temperature and in the presence of CF3COOH, SO2 undergoes Diels-Alder additions with (E)-1-acetoxybutadiene (8d) giving a 1:10 mixture of diastereomeric 6-acetoxysultines (9d + 10d). The Van't Hoff plot for equilibria 8d + SO2 reversible arrow 9d + 10d led to Delta H-r = -7.0 +/- 0.3 kcal/mol, Delta S-r = -42 +/- 3 cal . mol(-1) . K-1. At 20 degrees C, 8d underwent a slow cheletropic addition with SO2 giving 2-acetoxysulfolene (11d, Delta Hr congruent to -11.5 kcal/mol), the structure of which was established by single-crystal X-ray diffraction studies. (E)-Chloro (8e) and (E)-bromobutadiene (8f) did not undergo Diels-Alder additions with SO2, even in the presence of protic or Lewis acid promoters. Low yields of 2-chloro- (11e) and 8-bromosulfolene (11f) were obtained at 20 degrees C. The structure of 11e was confirmed by single-crystal X-ray diffraction. The potential energy hypersurfaces of the Diels-Alder and cheletropic additions of SO2 to butadiene (8a), (E)-piperilene (8b), (E)-1-methoxy- (8c), (E)-1-acetoxy- (8d), and (E)-1-chlorobutadiene (8e) were studied by ab initio quantum calculations at the MP2/6-31G* level. In agreement with the experiment, 6-substituted sultines 9X and 10X were less stable than the corresponding 2-substituted sulfolenes 11X for X = Me, OAc, Cl. With X = OMe, the two diastereomeric 6-methoxysultines (9c, 10c) and 8-methoxysulfolene (11c) were calculated to have similar stabilities. This is attributed to a stabilizing thermodynamic anomeric effect or gem-sulfinate/methoxy disubstitution effect in 9c, 10c. Such effects were not detected for sulfinate/acetoxy (9d, 10d) and sulfinate/chloro (9e, 10e) disubstitutions. The relative instability of 8-acetoxy- (11d) and 2-chlorosulfolene (11e) compared with their cycloaddents is attributed to repulsive interactions between the SO2 moieties and the 2-substituents. The Alder endo mode of [4 + 2] cycloaddition of SO2 is predicted to be faster than the "anti-Alder mode" of additions for dienes 8X, X = Me, OMe, OAc, Cl. The resulting diastereomeric sultines 9X and 10X, respectively, exist as equilibria (energy barrier: ca. 5-6 kcal/mol) of two conformers 9X reversible arrow 9X, 10X reversible arrow 10X. In general, the conformers 9X, 10X with pseudoaxial S=O group are preferred (conformational anomeric effect of the sulfinate moiety). Repulsive interactions between pseudoaxial S=O and polar cis-6-substituents (e.g.: X = OMe, OAc) in 9X may render conformers 9X (with the S-O and 6-X groups in pseudoequatorial positions) as stable as conformers 9X. The calculations predict the existence of conformational anomeric effects of 2-3 kcal/mol for the gem-sulfinate/methoxy (9c, 10'c) and gem-sulfinate/acetoxy disubstitution (9d, 10'd).

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Type
research article
DOI
10.1021/jo981679g
Author(s)
Fernandez, T.
Suarez, D.
Sordo, J. A.
Monnat, F.
Roversi, E.
de Castro, A. E.
Schenk, K.
Vogel, P.  
Date Issued

1998

Published in
The Journal of Organic Chemistry
Volume

63

Issue

25

Start page

9490

End page

9499

Subjects

Stereoselective synthesis

•

ab-initio

•

1

•

3-dienes

•

regioselectivity

•

gaussian-2

•

enthalpies

•

chemistry

•

energies

•

isoprene

•

carbon

Note

Univ Oviedo, Dept Quim Fis & Analit, E-33071 Oviedo, Spain. Univ Lausanne, Chim Sect, BCH Dorigny, CH-1015 Lausanne, Switzerland.

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REVIEWED

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EPFL

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LGSA  
Available on Infoscience
November 9, 2005
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/219732
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