American-Eurasian Journal of Scientific Research 2 (2): 161-169, 2007
ISSN 1818-6785
© IDOSI Publications, 2007
Corresponding Author: Dr. M.A.I. Salem, Synthetic Organic Chemistry Laboratory, Department of Chemistry, Faculty of
Science, Ain Shams University, Abbassiya, Cairo, Egypt
161
Utility of Cyanothioacetamide in the Synthesis of Pyrazolo [4, 3-c],
Isoxazolo [4, 5-c], Thieno [2, 3-b] and Furo [2, 3-c] of Thioxopyridine Derivatives
and their Antibacterial Activities
H.M.F. Madkour, M.A.I. Salem, M.I. Marzouk, M.E. Azab and N.F.H. Mahmoud
Synthetic Organic Chemistry Laboratory, Department of Chemistry,
Faculty of Science, Ain Shams University, Abbassiya, Cairo, Egypt
Abstract: The 4-oxo-2-thioxopyridines 2 and 6-oxo-2-thioxopyridines 3 have been synthesized via the
reaction of cyanothioacetamide and arylidenecyanoacetic ester. Thioxopyridines 2 was reacted with
acetic anhydride, hydrazine hydrate, chloroacetonitrile and sodium hypochlorite/ammonia to yield N, N-
diacetylpyridin-6-thione 4, pyrazolopyridin-6-thione 5, furopyridin-6-thione 6 and isoxazolpyridin-6-thione
7, respectively. Treatment of 6 with sodium ethoxide gave 8, while, reaction of 2 with ethyl chloroacetate
yielded 9 and 10 according to the reaction conditions. When 2 was allowed to react with POCl3/PCl5, it
afforded 13. Treatment of 9 with hydrazine hydrate furnished 11 which reacted with p-chlorobenzaldehyde
to yield 12. Reaction of 2 and 3 with methyl iodide produced 14 and 15 respectively. When hydrazine
hydrate was allowed to react with 15 it gave 16. Finally, boiling of 2 and 3 in cumene in the presence of
copper bronze yielded the disulfide derivatives 17 and 18 respectively. Biological screening of some new
synthesized compounds were determined in vitro using gram-positive and gram-negative bacterial
strains.
Key words: Cyanothioacetamide · thioxopyridine · pyrazolopyridine · isoxazolopyridine · furopyridine ·
thienopyridine · gram-positive and gram-negative bacterial strains
INTRODUCTION
A number of pyridone and thioxopyridine
derivatives have a widely medicinal and pharmaceutical
activities as anti-inflammation in rheumatism,
osteoposis, collagen diseases, bursitis, gout, anti-
parasitic, analgesic and muscular rheumatism [1-5],
fungicidal [6, 7] (specially in shampoos), insecticidal
[8], mammalian toxicity [9], neuromuscular stimulant
[10], antidepressant [11, 12], anticancer [13], antimobic
[14], antimalarial [15], antiviral [16], antihistaminic
agents [17, 18]. Also, these compounds are used as
irreversible Human Rhinovirus 3C protease inhibitor
[19], DNA-ligand bending [20], antituberculosis [21],
antitumor [22], antibacterial [23, 24] and antipyretic
agents [25]. On the other hand, some pyridine
derivatives are used to reduce lipids and cholestrol
levels in the blood [26], as treatment of unstable
angina [27], hair dyes [28], as X-ray contrast
media [1, 29], elastomer and ion exchange resins [30],
in floation process for recovery of metal concentrates
from metal bearing ores [31], as nitrogen stabilizer in
soil [32] and gyrase inhibitor [33].
RESULTS AND DISCUSSION
Within this respect, the aim of the present
work is to synthesise a wide derivatives of
thioxopyridine and study both the chemical
behaviour towards some chemical reagents and
biological activity towards some gram-positive and
gram-negative bacteria [34-36]. It has been
reported that cyanothioacetamide reacted with the
arylidene cyanoacetic ester in the presence of
triethylamine to give 3, 5-dicyano-6-oxo-4-phenyl-2-
thioxo-1, 2, 3, 4-tetrahydropyridine [37, 38] 1 as a
sole product while in our investigation we
isolated two products which are identified to be
(5E)-6-amino-5-arylidene-3-cyano-4-oxo-2-thioxo -2, 3,
4, 5-tetrahydropyridine 2 and (5E) 4-amino-5-
arylidine-3-cyano-6-oxo-2-thioxo -1, 2, 5, 6-
tetrahydropyridine 3.