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48 Combinatorial Chemistry & High Throughput Screening, 2015, 18, 48-52
Synthesis and Antitubercular Screening of Some Novel 4H-1,4-
Benzothiazines and their Sulfones Under Environment Benign Solvent
Free Conditions as Future Anti-Tubercular Agents
Anjali Guleria
*,1
, Dinesh K. Jangid
1
, Naveen Gautam
2
, Richa Lakhotia
3
, Abhay Chowdhary
3
and
Dinesh C. Gautam
1
1
Department of Chemistry, University of Rajasthan, Jaipur-302004, India
2
L.B.S Government PG College, Kotputli, Jaipur-303108, India
3
Department of Clinical Pathology, Haffkines Institute of Training, Testing and Research, Mumbai-
400 012, India
Abstract: Some novel analogs of 4H-1,4-benzothiazines were synthesized under environmentally
benign solvent free conditions by one pot oxidative cyclocondensation of substituted 2-
aminobenzenthiols with compounds having active methylene group and then converted in to
sulfones. These compounds were examined as antitubercular agents against Mycobacterium
tuberculosis H37Rv using REMA plate method. The best results have MICs from 6.4 to 8.8 µg/mL,
comparable to phenothiazines. IR, NMR and mass spectral investigations are included for structural
elucidation.
Keywords: 4H-1,4-benzothiazines, antitubercular agents, green chemistry, REMA, sulfones.
INTRODUCTION
Every third person in the world is infected with
Mycobacterium tuberculosis (Mtb). In the last few years, the
scenario got worse with increased cases of multi drug
resistant TB (MDR-TB) and extensively drug resistant TB
(XDR-TB). XDR-TB is increasing at alarming rate.
According to WHO’s latest report by September 2013, 92
countries had reported at least one XDR-TB case [1]. An
urgent need to design new anti-TB drugs that can treat MDR
and XDR-TB or at least shorten the treatment duration has
emerged because of draining pipeline of anti-TB drugs due
to MDR-TB which is resistant to first line drugs i.e. isoniazid
and rifampin and XDR-TB which is resistant to first line
drugs and half of the second line drugs e.g. any
flouroquinolone, amikacin, kanamycin, capreomycin, etc.
Phenothiazine drugs like chlorpromazine, thioridazine
and trifluoroperazine are reported to have antitubercular
activity [2] thus 4H-1,4-benzothiazines [3-9] can also be
anticipated as anti-Tb drugs because of their structural
resemblance to phenothiazines, in having fold along nitrogen
sulfur axis, a structural feature responsible for its wide
spectrum of pharmacological and biological activities [10-
14]. To explore this possibility for benzothiazines and its
derivatives we synthesized and screened some novel
compounds as antitubercular agents.
The mechanism of action like other psychotropic drugs
supposed to involve the direct binding of drug to type II
*Address correspondence to this author at the Department of Chemistry,
University of Rajasthan, Jaipur-302004, Rajasthan, India;
Tel: +919596931563; E-mail: anjali.guleria86@gmail.com
NADH dehydrogenase (NDH-2), a critical respiratory
enzyme of Mtb encoded by ndh gene [15], as an
uncompetitive inhibitor with respect to primary quinone
substrate, ubiquinone Q2 and non competitive inhibitor with
respect to NADH thus preventing the bacteria to respire
resulting in its growth inhibition as NDH-2 is likely to be the
only NADH-dehydrogenase enzyme utilized for growth in
an aerobic environment in the Mtb respiratory chain [16].
This paper concentrates on the synthesis of some novel
4H-1,4-benzothiazines under solvent free environmentally
benign conditions [17], their conversion in to sulfones [18-
20] and their screening as possible future anti-TB drugs by
REMA plate method. The structure elucidation has been
done by IR, NMR and mass spectroscopy.
MATERIALS AND METHODS
All the melting points were determined and are uncorrected.
Infrared spectra were recorded in KBr on SHIMADZU 8400 S
FTIR spectrophotometer.
1
H NMR and
13
C NMR spectra (by
broad band proton decoupling technique) were recorded in
DMSO-d6/CDCl3 on JEOL AL-300 spectrometer at
frequencies of (300.40 MHz and 75.45 MHz) respectively.
TMS (tetramethyl silane) is used as an internal standard and
Chemical shifts are measured in δ, ppm. Mass spectra were
recorded on JEOL SX 102/DA 600 using Xenon/Argon as FAB
(Fast Atom Bombardment) gas. The purity of compounds were
checked by TLC using silica gel "G" as adsorbent in various
non aqueous solvent systems and visualizing these by UV light
or in an Iodine chamber. Elemental analysis of these
compounds was also done.
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