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.
This work involves synthesis and characterization of some new 1, 3, 4-thiadiazole or pyrazoline derivatives heterocyclic containing indole ring. The new 2-amino-1, 3, 4-thiadiazole derivatives [IV] and [V] a, b were synthesized by cyclization reaction of 2-methyl-1H-indole-carbothiosemicarbazide [III] in H2SO4 acid or by reaction of indole-3-acetic acid or indole-3-butanoic acid with thiosemicarbazide in the presence of phosphorous oxychloride, respectively. Amide derivatives [VI]-[VIII] were synthesized by the reaction equimolar of 2-amino-1, 3, 4-thiadiazoles and (acetyl chloride, benzoyl chloride, anisoyl chloride and heptanoyl chloride) in DMF and pyridine as accepter. The new pyrazolone derivatives [XI] a, b were synthesized from heati
... Show MoreSeveral azo dyes were synthesized through coupling reaetion of some substituted phenols and B.naphthol with diazonium salt of 2- amino-1,3-4- thiadiazol -5- thiol. All the synthesized compounds during this work were characterized using some speetral data (F.TIRand UV)andM.P . 2-[4 --Hydroxy napthyl-azo ] -1,3,4-Thiadiazol -5-Thiol • 2- [2-- hydroxy –4- NO2 – phenyl- azo]- 1,3,4 - Thiadiazol –5-Thiol. • 2- [3--Amino-4-Hydroxy phenyl –azo]-1,3,4 - Thiadiazol –5-Thiol. . • 2-[2--Amino-4-Hydroxy phenyl -azo]-1,3,4 - Thiadiazol –5-Thiol . • 2- [3--Amino-6- Hydroxy phenyl -azo]-1,3,4 - Thiadiazol –5-Thiol. • 2-[2-- Hydroxy- 5 – chloro – Pheny - azo]- 1,3,4 - Thiadiazol –5-Thiol . • 2- [4-- Hydroxy phenyl -azo] -1,
... Show MoreThe research included the preparation of cyclic compounds from thiazoles, imidazoles and oxazepines from the reaction of cyclization starting material that acts Schiff bases, which is a raw material in the formation of cyclic compounds from Schiff's(B1) by reaction of 4- aminobenzenesulfonylamide with 4-hydroxyacetophenone which can used to synthesized two lines. The first introducing the preparation of pyrazoles [B4, B5] from ester [B2], which derived to acid hydrazide[B3] with hydrazine hydrate and final pyrazoles obtained by the reaction with diethylmalonate and acetylacetone. The second including prepared the new 1,3-oxazepine1,5-dione derivatives[B6,B7,B8] from adding different anhydrides to the base[B1] as a seven membered ring ; te
... Show MoreIn this research, the theme for employing a simple and sensitive method is to employ a new Schiff base ligand (N’-(4- (dimethyl amino) benzylidene)-3, 5-dinitrobenzohydrazide) to estimate Ni (II) to form orange complex (N-(4-(dimethyl amino) benzylidene)-3, 5-dinitrobenzohydrazide nickel (II) chloride) in acid medium (hydrochloric acid), it gives an absorption peak at the wavelength 485 nm. The preferred conditions were studied to form the complex and obtain the highest absorbance including concentration of Schiff base ligand, the best medium for complex formation, effects of addition sequence on complex formation, the effect of temperature on the absorbance of the complex formed, and the setting time of the formed complex. The obtained r
... Show MoreTwo series of Schiff Bases [VI]n and thiazolidin-4-one derivatives[VII]n were synthesized by many steps starting from cyclization of 4- hydroxyacetophenon with thiourea in iodine to yield 1,3-thiazole compound which was reacted with pentoxy bromide in anhydrous potassium carbonate to converted compound[II] and this reacted with Phenol to yield azo compound[III]. The azo compound reacted with ethyl chloro acetate in basic medium to get a new easter compound[IV] which is converted to their acid hydrazid[V]. The later compound condensation with n-alkoxy benzaldehyde to give new Schiff bases[VI]n . Imine group undergoes addition cyclization with thioglycolic acid to get thiazolidinone compounds[VII]n .Also, two new series of Schiff Bases [XII]n
... Show MoreThe crystal structures of a new polymorph and seven new derivatives of 2-(1-phenyl-1H-1,2,3-triazol-4-yl)pyridine have been characterized and examined along with three structures from the literature to identify trends in their intermolecular contact patterns and packing arrangements in order to develop an insight into the crystallization behaviour of this class of compound. Seven unique C-H...X contacts were identified in the structures and three of these are present in four or more structures, indicating that these are reliable supramolecular synthons. Analysis of the packing arrangements of the molecules using XPac identified two closely related supramolecular constructs that are present in eight of the 11 structures; in all cases, the st
... Show MoreA simple, rapid and sensitive spectrophotometric method has been proposed for the determination of La (III) using 3-hydroxy -4-(2-hydroxy-phenyl azo) naphthalene -1- sulfonic acid as a chromogenic reagent. This method is based on the formation of a red-pink colored complex, upon the reaction of La(III) with the reagent in an alkaline medium (pH= 9.50), having a maximum absorbance at 459 nm. Beer's law is valid in the concentration range 0.512 µg.ml-1 with a Sandell's sensitivity value of 0.0188 µg.cm-2 and molar absorptivity of 7376.12 L.mol-1.cm-1. The stoichiometric composition of the chelate is 1:3. The effect of the presence of different cations as interferants in the determination of La(III) under the given optimum conditions wer
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