Regioselective synthesis of functionalized 1,4-benzothiazines via intramolecular SNArF and SNArH cyclizations

In the preparation of 1,4-benzothiazines, intramolecular nucleophilic aromatic substitution (S N Ar) cyclizations of thiol-bearing fluoro-nitroanilines exhibited unexpected regioselectivity preferences. Microwave-assisted heating facilitated ring closure but did not alter the intrinsic regiochemical bias. Both standard S N Ar F and a vicarious nucleophilic substitution of hydrogen (S N Ar H ) reactions led to an undesired 1,4-benzothiazine substitution pattern. Frontier molecular orbital (FMO) analysis revealed substantial LUMO polarization at the C-2 position irrespective of fluorine versus hydrogen substitution at this site, providing a mechanistic rationale for the observed regioselectivity. Guided by these insights, a symmetrical dinitro-activated substrate was used to overcome the intrinsic electronic bias and enable access to the desired 1,4-benzothiazinedioxides in a concise seven-step sequence. The selectivity of the final N -carbamoylation step was determined by 13 C NMR chemical shift calculations. This work addresses regioselectivity challenges in benzothiazine synthesis and highlights the power of combining experimental and computational analyse. • A rare S N Ar H reaction. • A computational analysis that provides a rationale for the experimentally observed intrinsic regiochemical preferences. • Strategic substrate design that overcomes the substituent effect bias and enables a controlled access to the desired heterocyclic framework. • General insights into regioselectivity control in intramolecular aromatic substitution reactions that should inform the rational design and synthesis of related heterocyclic systems.

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Publication Details

Journal
Tetrahedron Letters
Published
2026-03-14
DOI
https://doi.org/10.1016/j.tetlet.2026.156040
Primary Topic
Catalytic C–H Functionalization Methods
Type
article
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article

Regioselective synthesis of functionalized 1,4-benzothiazines via intramolecular SNArF and SNArH cyclizations

Peter Wipf, Clare Hill
Tetrahedron Letters
Catalytic C–H Functionalization Methods
article

Regioselective synthesis of functionalized 1,4-benzothiazines via intramolecular SNArF and SNArH cyclizations

Peter Wipf, Clare Hill
article en

Abstract

In the preparation of 1,4-benzothiazines, intramolecular nucleophilic aromatic substitution (S N Ar) cyclizations of thiol-bearing fluoro-nitroanilines exhibited unexpected regioselectivity preferences. Microwave-assisted heating facilitated ring closure but did not alter the intrinsic regiochemical bias. Both standard S N Ar F and a vicarious nucleophilic substitution of hydrogen (S N Ar H ) reactions led to an undesired 1,4-benzothiazine substitution pattern. Frontier molecular orbital (FMO) analysis revealed substantial LUMO polarization at the C-2 position irrespective of fluorine versus hydrogen substitution at this site, providing a mechanistic rationale for the observed regioselectivity. Guided by these insights, a symmetrical dinitro-activated substrate was used to overcome the intrinsic electronic bias and enable access to the desired 1,4-benzothiazinedioxides in a concise seven-step sequence. The selectivity of the final N -carbamoylation step was determined by 13 C NMR chemical shift calculations. This work addresses regioselectivity challenges in benzothiazine synthesis and highlights the power of combining experimental and computational analyse. • A rare S N Ar H reaction. • A computational analysis that provides a rationale for the experimentally observed intrinsic regiochemical preferences. • Strategic substrate design that overcomes the substituent effect bias and enables a controlled access to the desired heterocyclic framework. • General insights into regioselectivity control in intramolecular aromatic substitution reactions that should inform the rational design and synthesis of related heterocyclic systems.

Tetrahedron LettersVol. 179
University of Pittsburgh (US)
Openalex Percentile: Top 21%
Catalytic C–H Functionalization Methods
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