Nemzeti Gyógyszerkutatási és Fejlesztési Laboratórium (PharmaLab)(RRF-2.3.1-21-2022-00015)
Támogató: NKFIH
Thiourea and structurally related urea derivatives are widely recognised for their
ability to transport anions through hydrogen bonding interactions. The strength of
these interactions correlates with the electronegativity of the ligand and the acidity
of the NH hydrogens involved. Thiourea, being more acidic than urea, exhibits partial
deprotonation in the presence of certain anions such as organic carboxylates, fluoride,
and bromide, while remaining resistant to deprotonation by chloride. This behaviour
suggests a degree of selectivity toward chloride ions. Additionally, while carbamide-containing
molecules tend to aggregate—potentially reducing their ion-binding efficiency—thiourea
derivatives show reduced aggregation, preserving their binding capabilities. In this
study, we report the synthesis and characterisation of 21 novel thiourea derivatives
obtained by reacting 2-aminobenzoylamino acid esters with various substituted phenyl
isothiocyanates. Seven similar thiourea-containing molecules were made as a comparison—without
the amino acids—by reacting aniline with the different phenyl isothiocyanates. The
reaction kinetics were found to be influenced primarily by the electronic nature of
the substituents on the phenyl ring. Electron-withdrawing groups (EWGs), such as para-nitro,
3,5-bis(trifluoromethyl), and fluorine, accelerated the reaction, while electron-donating
groups (EDGs), such as para-methoxy, slowed it down. Interestingly, the nature of
the amino acid precursors had no significant impact on reaction time; however, reactions
with aniline proceeded the fastest. Solvent choice also played a role: reactions in
N,N-dimethylformamide (DMF) proceeded faster than in acetone, although with reduced
yields. Consequently, reaction conditions were optimised to balance time efficiency
and product yield. To evaluate the chloride ion-binding properties of the synthesised
compounds, 1H NMR titration experiments were conducted in deuterated dimethyl sulfoxide
(DMSO-d6). The association constants (Ka) derived from these studies revealed a clear
correlation with the electronic nature of the substituents. Compounds bearing EWGs
exhibited enhanced chloride binding, while those with EDGs showed diminished binding
affinity. Surprisingly, the presence of amino acid moieties led to a decrease in Ka
values, despite the electron-withdrawing nature of the amide groups. This suggests
that steric or conformational factors may play a role in modulating binding strength.
Overall, the synthesised thiourea derivatives demonstrate mild, reversible chloride
ion-binding behaviour, making them promising candidates for further development as
selective anion receptors. The insights gained from this study contribute to a deeper
understanding of structure–activity relationships in anion-binding systems and may
inform the design of future supramolecular architectures with tailored ion recognition
properties.