1233
ISSN 1063-7745, Crystallography Reports, 2021, Vol. 66, No. 7, pp. 1233–1237. © Pleiades Publishing, Inc., 2021.
Synthesis and Crystal Structure Analysis of 3,3'-[(3-Sulfanyl
Phenyl)Methylene]Bis(4-Hydroxy-2H-1-Benzopyran-2-One) :
5-Methyl-1,3-Thiazol-2(3H)-Imine
G. Sharma
a
, S. Anthal
a
, M. B. Deshmukh
b
, P. P. Mohire
b
, T. R. Bhosale
b
,
C. Sudarsanakumar
c
, and R. Kant
a,
*
a
X-ray Crystallography Laboratory, Department of Physics, University of Jammu, Jammu Tawi, 180006 India
b
Department of Chemistry, Shivaji University, Kolhapur, 416004 India
c
School of Pure and Applied Physics, Mahatma Gandhi University, Kottayam, 686560 Kerala
* e-mail: rkant.ju@gmail.com
Received August 29, 2020; revised March 31, 2021; accepted March 31, 2021
Abstract—The structure of 3,3'-[(3-sulfanylphenyl)methylene]bis(4-hydroxy-2H-1-benzopyran-2-one) :
5-methyl-1,3-thiazol-2(3H)-imine was determined by X-ray crystallography. It crystallizes in the mono-
clinic crystal system with space group Cc. The unit cell parameters are: a = 20.1008(12) Å, b = 15.2487(9) Å,
c = 8.3462(4) Å, β = 92.86(2)°, and Z = 4. The crystal structure has been solved by using direct methods and
refined by full matrix least squares procedures to a final R-factor of 0.040 (wR(F
2
) = 0.097) for 5152 observed
reflections. The bond angles around the chromene moieties are almost identical but deviate significantly from
the values observed in some analogous structures. There exists few C–H⋅⋅⋅O/O–H⋅⋅⋅O intramolecular hydro-
gen interactions, besides intermolecular interactions of the type N–H⋅⋅⋅O, S–H⋅⋅⋅N, O–H⋅⋅⋅N, and C–H⋅⋅⋅S,
respectively.
DOI: 10.1134/S1063774521070166
INTRODUCTION
Chromene derivatives are important intermediates
in various naturally occurring substances such as alka-
loids, anthocyanins, polyphenols, tocopherols and
flavonoids [1]. Many substituted 2-aminochromene
derivatives have been utilized in cosmetic and pigment
industry [2]. Lonchocarpin is another natural
chromene with yellow orange crystals which is isolated
from the ether extract of seeds and roots of Lonchocar-
pus scericeus [3]. Fused chromene scaffolds have also
several relevance’s in heterocyclic chemistry field [4]
such as anticancer [5–9], anti-tuberculotic [10], anti-
microbial [11], anti-inflammatory [12], antioxidant
[13], analgesic [14], antimalarial [15], and anti-HIV
[16] activities. The 2H-chromene nucleus also present
in health promoting agents like polyphenols [17] and
are a favoured scaffold found in many biologically
active molecules [18–20]. 4-Hydroxy benzopyran 2-one
acts as an anticoagulant for the treatment of thrombo-
embolic conditions. The anticoagulant activity of bis-
benzopyran results from inhibition of a vitamin K-
dependent step in the hepatic synthesis of clotting fac-
tors II (prothrombin). The presence of thiazole moiety
enhances the fibrinogen receptor antagonists with
antithrombotic activity [21]. Therefore, the synthesis
and structural characterization of the title compound
was undertaken.
EXPERIMENTAL
Synthesis
A mixture of 4-hydroxycoumarin (1 mmol) and
3-mercapto benzaldehyde (1 mmol), with 5 mL
LTTM was taken in a 50 mL round bottomed flask and
srirred at room temperature to get Knoevenagel prod-
uct, monitored by TLC and then 2-amino 5-methyl
1,3-thiazole (1 mmol) were added and the same reac-
tion mixture further ref luxed for 20 min. The progress
of the reaction was monitored by TLC using petro-
leum ether –ethyl acetate (8 : 2 ) then cooled to
room temperature. The solid product formed was col-
lected by simple filtration, washed with ethanol and
diethyl ether. Finally, the crude product was recrystal-
lized from ethanol to obtain the pure crystalline prod-
uct. Yield: 55%, m.p.: 206°C. The reaction scheme of
the compound is shown in Fig. 1.
Yield, 55%, m.p. 206°C; IR (v
max
) cm
–1
: 3400–
3300 (SH), 3250 (NH), 2920 (C–H), 1668 (C=O), 1604
(C=C);
1
H NMR (DMSO-d
6
) : δ (ppm) 2.15 (3H, s,
CH
3
), 4.8 (1H, s, NH of thiazole ring), 6.2 (1H, s, CH
benzylic proton), 6.8–8.1 (13H, m, aromatic protons
v/v
STRUCTURE OF ORGANIC
COMPOUNDS