In this work pyrazolin derivatives were prepared from the diazonium chloride salt of 4-aminobenzoic acid. Azo compounds were prepared from the reaction of an ethanolic solution of sodium acetate and calculated amount of active methylene compound namely, acetyl acetone to obtain the corresponding hydrazono derivative (1). Cyclocondensation reaction of compounds (1) with hydrazine hydrate and phenyl hydrazine in boiling ethanol affording the corresponding pyrazoline-5-one derivatives of 4-aminobenzoic acid (2,3). Then compound (3) was reacted with thionyl chloride to give the corresponding acid chloride derivative(4), followed by conversion into the corresponding acid hydrazide derivative (5) carboxylic acid thiosemicarbazide (11), esters (14,15), thioesters (16,17) and amides (18,19), when treated hydrazine hydrate, thiosemicarbazide, alcohols, alkylthiol and secondary amines in dry refluxing benzene; respectively. Schiff's bases (6-8) were prepared by refluxing of compound (5) with different aldehydes and ketons, then two compounds from the Schiff's bases were cyclized with ?-mercapto acetic acid to give (9 and 10). Furthermore, 1,2,4-triazole derivative (12) have been also prepared by refluxing thiosemicarbazide derivative with sodium hydroxide solution (4%) followed acidification of the result using (10%)hydrolic acid. Moreover, a thiadiazole derivative (13) has been prepared by treatment of thiosemicarbazide derivative with concentrated sulfuric acid as cyclyzing agent. Finally, oxadiazole derivative (20) has prepared by condensation of its acid hydrazide derivative with carbon disulfide in basic medium.
The 4-(?-bromo acetyl)-4?-toluene sulfonanilide (2) was used as key intermediate to synthesize new heterocyclic compounds. This bromo compound was synthesized via sulfonation of amino group of p-amino acetophenone using Hinsburg method with 4-toluene sulfonyl chloride to form 4-acetyl-4?-toluene sulfonanilide (1) which is used as a starting material in this work. This compound was brominated to yield compound (2) which is used as a precursor to synthesize new five and seven membered heterocyclic compounds such as substituted 1,3-oxazoles (3,4), 1,3-thiazole derivatives (5-7), thiourea compounds (8a,b), 1,3-Thiazoline-2-thione compounds (9a-f) and 1,2,5-triazepine compounds (11a-d). The synthesized compounds were identified depending u
... Show MoreThis work is based on the synthesis of Cobalt(II) and Cadmium(II) mixed-ligands compounds obtained from the reaction of N'-(4-methylsulfanyl-benzoyl)-hydrazine carbodithioic acid methyl ester as a ligand and using ethylendiamine (en), 2,2'-bipyridine (bipy) or 1,10-phenanthroline (phen) as a co-ligand. The synthesis of ligand (HL) was based on multi-steps synthetic procedure. The reaction of 4-methylsulfanyl-benzoyl chloride with hydrazine gave 4-methylsulfanyl-benzoic acid hydrazide. This compound was reacted with carbon disulfide and potassium hydroxide in methanol to yield N'-(4-methylsulfanylbenzoyl)-hydrazine potassium thiocarbamate, which upon reaction with methyl iodide resulted in the formation of the ligand. A range of physico-chem
... Show MoreThis work is based on the synthesis of Cobalt(II) and Cadmium(II) mixed-ligands compounds obtained from the reaction of N'-(4-methylsulfanyl-benzoyl)-hydrazine carbodithioic acid methyl ester as a ligand and using ethylendiamine (en), 2,2'-bipyridine (bipy) or 1,10-phenanthroline (phen) as a co-ligand. The synthesis of ligand (HL) was based on multi-steps synthetic procedure. The reaction of 4-methylsulfanyl-benzoyl chloride with hydrazine gave 4-methylsulfanyl-benzoic acid hydrazide. This compound was reacted with carbon disulfide and potassium hydroxide in methanol to yield N'-(4-methylsulfanylbenzoyl)-hydrazine potassium thiocarbamate, which upon reaction with methyl iodide resulted in the formation of the ligand. A range of physico-c
... Show MoreOur work included a synthesis of three new imine derivatives—1,3-thiazinan-4-one, 1,3-oxazinan-6-one and 1,3-oxazepin-4,7-dione—which contained an adamantyl fragment. These were produced via the condensation of the Schiff`s base (E)-N-(adamantan-1-yl)-1-(3-aryl)methanimine with 3-mercaptopropanoic acid; 3-chloropropanoic acid; and maleic, citraconic anhydride, respectively. These new imines were prepared via the condensation of adamantan-1-ylamine and 3-nitro-, 3-bromobenzaldehyde in n-BuOH. We obtained a good yield of products. FTIR, 1H NMR spectroscopy and C.H.N.S analysis were used to diagnostic the products. The molecular structure of (E)-N-(adamantan-1-yl
... Show MoreReaction of  p-fluoro benzoic acid with the thiosemicarbazide and salcialdehyde gave the new bidentate ligand .The prepared ligand Identified by FT-I.R and U.V-Visible spectcopic technique .Treatment of the prepared   ligand   with following metal ions  M=Tb(III),Eu(III),Nd(III) and La(III) ,in ethanol with a (1:1) M:L ratio and at pH=7 yielded series of neutral complexes as the general formula  [M LCl (H O ]. The prepared complexes were characterized using (FT-IR, UV-Vis) spectra , melting point, molar conductivity measurements . chloride ion content were also evolution by (mhor method) . The proposed structure of the complexes using program , chem office 3D(2004) .
The purpose of this research is to prepare new vanillic acid derivatives with 1,2,4-triazole-3-thiol heterocyclic ring and evaluate their antimicrobial activity in a preliminary assessment. A multistep synthesis was established for the preparation of new vanillic acid-triazole conjugates. The intermediate of 4-(4-amino-5-mercapto-4H-1,2,4-triazol-3-yl)-2-methoxyphenol (4) reacts with different heterocyclic aldehydes (thiophene-2-carboxaldehyde, pyrrole-2-carboxaldehyde, thiophene-3-carboxaldehyde, and furfural ) in ethanol containing few drops of acetic acid yielded the corresponding 4-(4-(substituted amino)-5-mercapto-4H-1,2,4-1triazol-3-yl)-2-methoxy phenol derivatives (
The new schiff bases derived from D-erythroascorbic acid contaning heterocyclic unit were synthesized by condensation of D-erythroascorbic acid with aromatic amine (containing 1,3,4oxadiazole or 1,3,4-thiadiazole unit) in dry benzene using glacial acetic acid as a catalyst. Derythroascorbic acid [IV] was synthesized by four steps (Scheme 1), while the primary aromatic amine which is containing 1,3,4-oxadiazole [VII] or 1,3,4-thiadiazole [VIII] synthesized by the reaction of 4methoxy benzoyle hydrazine [VI] with 4-amino benzoic acid or by the reaction tuloic acid with thiosemicarbazide, respectively in the presence of POCl3. The new 1,3-oxazepine derivatives were obtained by addition reaction of Schiff bases with d
... Show MoreThe aim of this work is the synthesis of new derivatives of barbiturate of D-erythroascorbic acid. To obtain these derivatives, the 5,6-O-isopropylidene-L-ascorbic acid (4) was chosen, which was prepared from the reaction of L-ascorbic acid (3) as a starting material with dry acetone in the presence of hydrogen chloride. The esterification of hydroxyl groups at C-2 and C-3 positions with excess of benzoyl chloride in dry pyridine was obtained compound (5). Hydrolysis for compound (5) in acetic acid (65%) gave the compound (6). Oxidation of the product (6) with sodium periodate results an Al
... Show MoreNewly 4-amino-1,2,4-triazole-3-thione ring 2 was formed at position six of 2-methylphenol from the reaction of 6-(5-thio1,3,4-oxadiazol-2-yl)-2-methylphenol 1 with hydrazine hydrochloride in the presence of anhydrase sodium acetate. Seven newly fused heterocyclic compounds were synthesized from compound 2. First fused heterocyclic was 6-(6-(3,5-di-tertbutyl-4-hydroxyphenyl)-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazol-3-yl)-2-methylphenol 3 synthesized from reaction compound 2 with 3,5-di-tert-butyl-4-hydroxybenzoic acid in POCl3. Reaction compound 2 with bromophencylbromide afford 6-(6-(4-bromophenyl)-5H-[1,2,4]triazolo[3,4-b][1,3,4]-thiadiazin-3-yl)-2-methylphenol 4. 6-(6-thio-1,7a-dihydro-[1,2,4] triazolo[3,4-b][1,3,4]-thiadiazol-3-yl)-2
... Show MoreA novel metal complexes Cu (II), Co (II), Cd (II), Ru (III) from azo ligand 5-((2-(1H-indol-2-yl)
ethyl) diazinyl)-2-aminophenol were synthesized by simple substitution of tryptamine with 2-aminophenol.
Structures of all the newly synthesized compounds were characterized by FT IR, UV-Vis, Mass spectroscopy
and elemental analysis. In addition measurements of magnetic moments, molar conductance and atomic
absorption. Then study their thermal stability by using TGA and DSC curves. The DCS curve was used to
calculate the thermodynamic parameters ΔH, ΔS and Δ G. Analytical information showed that all complexes
achieve a metal:ligand ratio of [1:1]. In all complex examinations, the Ligand performs as a tri