FULL PAPER
DOI: 10.1002/ejoc.201301710
One-Pot Synthesis of 2-Imino-4-(trifluoromethyl)thiazolidin-4-ol Derivatives in
a Three-Component Reaction: Application to Structurally Diverse Scaffolds of
Biological Interest Through Subsequent Reactions
Tulshiram Dalmal,
[a]
K. Appalanaidu,
[a]
Umesh B. Kosurkar,
[a]
N. Jagadeesh Babu,
[b]
and
Ravindra M. Kumbhare*
[a]
Keywords: Medicinal chemistry / Multicomponent reactions / Cyclization / Nitrogen heterocycles / Sulfur heterocycles /
Fluorine
A highly efficient method for the synthesis of 2-imino-4-(tri-
fluoromethyl)thiazolidin-4-ol derivatives has been achieved
by the one-pot, three-component reactions of primary
amines, aryl isothiocyanates, and 3-bromo-1,1,1-trifluoro-
Introduction
There has been increasing interest in the introduction of
fluorine or a fluorinated group into organic compounds,
since this influences the pharmacodynamic and pharmaco-
kinetic properties of a drug.
[1]
The introduction of a tri-
fluoromethyl group into cyclic compounds, especially at
strategic positions of drug molecules, has become an impor-
tant aspect of pharmaceutical research, owing to the unique
physical and biological properties of fluorine.
[2,3]
Therefore,
the development of fluorinated potential drugs is a key is-
sue and a challenge for medicinal chemistry and related dis-
ciplines.
[4]
2-Imino-1,3-thiazolidines and 2-imino-1,3-thiaz-
olines have emerged as important classes of heterocyclic
compounds, due to their diverse applications in medicinal
chemistry.
[5,6]
These heterocycles show a wide range of bio-
logical properties, including anti-inflammatory, anodyne,
anti-Alzheimer, antimicrobial, antihistaminic, antihyperten-
sive, anticonvulsant activities, and also as myeloperoxidase
inhibitors etc.
[7,8]
For example, 4,5-dialkyl-substituted thi-
azolidines I (Figure 1) are reported to be nitric oxide syn-
thase inhibitors.
[9]
A member of another class of thiazolid-
ines, 3-methylthiazolidine II (Figure 1; R
1
= H, R
2
= Me),
is a potent inhibitor of indole–ethylamine N-methyltrans-
ferase.
[10]
β-(Hydroxyethyl)thiazolidines III (Figure 1) are
reported to be effective antihypertensive agents.
[11]
2-(Tetra-
[a] Fluoroorganic Division, Indian Institute of Chemical
Technology, CSIR,
Hyderabad, India
E-mail: kumbhare@iict.res.in, rakumbhare@yahoo.com
http://www.iictindia.org/
[b] Laboratory of X-ray Crystallography, Indian Institute of
Chemical Technology, CSIR,
Hyderabad, India
Supporting information for this article is available on the
WWW under http://dx.doi.org/10.1002/ejoc.201301710.
© 2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim Eur. J. Org. Chem. 2014, 2468–2479 2468
propanone. The reactions go via symmetrical and unsymmet-
rical thiourea intermediates. Subsequent reactions of the
products allow the synthesis of various scaffolds, including
isoxazoles, triazoles, and propargylamine derivatives.
hydronaphthalen-1-yl)iminothiazolidine IV (Figure 1) acts
as an antidepressant.
[12]
3-Substituted 2-(cyanoimino)-
thiazolidines V (Figure 1) can be used in agriculture, due to
their neonicotinoid insecticidal activity, and thiacloprid (V :
R = H) is a commercially available insecticide released by
Bayer in 2001.
[13]
Figure 1. Biologically active 2-imino-1,3-thiazolidine motifs.
Furthermore, thiazoline derivatives have applications in
agriculture as pesticides, acaricides, insecticides, and plant-
growth regulators.
[14]
Consequently, in recent decades, there
has been continuous interest in developing new synthetic
strategies for the synthesis of such attractive target mo-
lecules.
A detailed literature survey revealed the various methods
available for the synthesis of functionalized 2-iminothiazol-
idines and related compounds. These include acid-mediated
intramolecular cyclization of N-(2-hydroxyethyl)thiourea,
ring transformation of 2-(thiocyanomethyl)aziridines, treat-
ment of aziridines with thiocyanuric acid, reaction of 2-vin-
ylaziridine with phenyl isothiocyanate, condensation of α-
halo ketones with thioureas, etc.
[15,16]
However, methods for
the synthesis of 2-imino-1,3-thiazolidin-4-ol derivatives are