الفهرس 
IntroductionOnly 14 pages are availabe for public view
 |  | from | 305 |  |  |
| | | from | 305 | | |
Abstract
This thesis Synthesis and studying the chemical behaviour phthalazinone derivatives, Study the complex of the radioactive element with application to isolate radioactive element such as uranium and the biological activity of complex.
Thesis consists of the following part:
1- Summary
2- Introduction
In this section brief of literatures review of the different methods of preparation and reaction of phthalazine derivatives , complexes and way of methods of separation of uranium ions .
3- Results and Discussion
The experimental methods Explain the synthesis of the designed compounds as well as their different methods applied for characterization of new compounds and separation technique.
Schemes (1-5) illustrate the synthetic pathways followed in the preparation of target compounds.
In this part the synthesize of N-substituted-4-(3-chloro-4 methylphenyl)phthalazin-1-ones derivatives with the aim of information about the reaction , nuclear application and the biological activities of these molecules with differentiation of the molecules and there complex .
4-(3-Chloro-4-methylphenyl)phthalazin-1(2H)-one (2) was prepared from 2-(3-chloro-4-methylbenzoyl) benzoic acid (1) that produced from Friedel–Crafts acylation reaction of phthalic anhydride and 2-chlorotoluene and the interaction with hydrazine hydrate in ethanol under thermal reflux and 2,2-thiocarbonylbis(4-(3-chloro-4-methylphenyl)phthalazin)-1(2H)-one (3) and 6-( 3-chloro-4-methylphenyl) –[1,2,4]triazolo[3,4-a] phthalazine -3(2H)thione (4) was synthesize by reaction of 2-(3-chloro-4-methylbenzoyl) benzoic acid (1) and thiocarbonic dihydrazide in different solution.
Reaction with ethyl chloroacetate
When 4 substituted phthalazin-1(2H)-one (2) was submitted to react with carbon electrophiles ethyl chloroacetate in the dry acetone and anhydrous potassium carbonate under reflux yielded ethyl 2-(4-(3-chloro-4-methylphenyl)-1-oxophthalazin-2(1H)-yl)acetate (5)
Reaction with halide monosaccharide
the phthalazin-1(2H)-one (2) react with α-D-arabino- and gluco-pyranosyl produce the N-cyclonucleosides 2-(α-D-arabino- and/or gluco-pyranosyl)-4-phenyl phthalazin-one (6 and 7).
Reaction with amino acids
Reactions of the phthalazinone (2) react with halide of amino acid to yielded α-amino acids carrying phthalazinone (8).
Reaction with benzoyl chloride.
Phthalazin-1(2H)one derivative 2 was react with benzoyl chloride in boiling dry acetone in presence of anhydrous potassium carbonate yielded benzoyl-4-(3-chloro-4-methylphenyl)phthalazin-1(2H)-one (9).
Reaction with allylbromide:
The Phthalazin-1(2H)one derivative 2 was submit to react with allylbromide in boiling dry acetone in presence of anhydrous potassium carbonate yielded 2-allyl-4-(3-chloro-4-methylphenyl)phthalazin-1(2H)-one (10).
Reaction with 2-choroethanol :
Phthalazin-1(2H)-one derivative 2 interact with 2-chloroethanol in the dry acetone as solvent and anhydrous potassium carbonate to produce 4-(3-chloro-4-methylphenyl)-2-(2-hydroxyethyl)phthalazin-1(2H)-one (11).
Reaction with phenyl isothiocyanate :
The reaction of 4-(3-chloro-4-methylphenyl)phthalazin-1(2H)-one 2 with phenyl isothiocyanate in boiling benzene yield 4-(3-chloro-4-methylphenyl)-1-oxo-N-phenylphthalazine-2(1H)-carbothioamide (14).
Reaction with ethyl cyanoacetate:
The compound 2 react with the ethyl cyanoacetate in boiling ethanol to yield (2)-ethyl 3-amino-3-(4-(3-chloro-4-methylphenyl)-1-oxophthalazin-2(1H)-yl)acrylate (15) the reaction take place via nucleophilic addition on cyano group not via tetrahedral nucleophilic substitution at acyl moiety
Reaction with piperidine under Mannich reaction :
The compound 2 was submitted to react with piperidine and formaldehyde in presence of few drops of hydrochloric acid to produce 4-(3-chloro-4-methylphenyl)-2-((piperidin-1-yl)methyl)phthalazin-1(2H)-one (17).
Reaction with ethanol amine :
The compound 2 react with the ethanolamine in oil bath to yield 2-(2-aminoethyl)-4-(3-chloro-4-methylphenyl)phthalazin-1(2H)-one (19)
Reaction with epichlorohydrine:
Reaction of phthalazin-1(2H)-one 2 with epichlorohydrine in boiling dry acetone in the presence of anhydrous potassium carbonate to yield 4-(3-chloro-4-methylphenyl)-2-((oxiran-2-yl)methyl)phthalazin-1(2H)-one (24) .
Reaction with hydrazine hydrate
The reaction of phthalazin-1(2H)-one ester (5) react with hydrazine hydrate in boiling ethanol afforded 2-(4-(3-chloro-4-methylphenyl)-1-oxophthalazin-2(1H)-yl)acetohydrazide (28).
Metal complex of phthalazin-1(2H)-one:
The metal complex of compound (2,5 and 24) is formed by separately dissolved of small amount in the 10 ml of acetic acid then diluted by chloroform up to 50ml Stranded solution 100ppm of uranyl nitrate (UO2(NO3)26H2O) were separately dissolved added 1:1 volume of of uranyl nitrate solution was added to the 1 The mixtures were stirred together in water bath for 30 min.
Ore used as uranium source
the present case study in extraction of uranium from hydrophilic residue (P2O5 48.10%, 500 ppm and many other impurities) .
Extraction of uranyl ion by Use of prepared organic compounds in the liquid-liquid extraction
A novel ligand 4-(3-chloro-4-methylphenyl)phthalazin-1(2H)-one (2) ethyl 2-(4-(3-chloro-4-methylphenyl)-1-oxophthalazin-2(1H)-yl)acetate (5) and 4-(3-chloro-4-methylphenyl)-2-((oxiran-2-yl)methyl)phthalazin-1(2H)-one (26) used as ligand and complex structure was determined with uranium as heavy metal
Extraction of uranyl ion from standard solution
Extraction of uranyl ion by using 4-(3-chloro-4-methylphenyl)phthalazin-1(2H)-one (2) solvent.
Extraction of uranyl ion by using ethyl 2-(4-(3-chloro-4-methylphenyl)-1-oxophthalazin-2(1H)-yl)acetate (5) solvent .
Extraction of uranyl ion by using 4-(3-chloro-4-methylphenyl)-2-((oxiran-2-yl)methyl)phthalazin-1(2H)-one (26) solvent.
Selective separation of uranium from raffinate phosphoric acid dissolved in Nitric acid
The phthalazinone derivatives was used to extract uranium from the raffinate phosphoric acid produced from the industrial process of the of phosphoric acid food greed production the raffinate was dissolved in 6 molar HNO3
Selective separation of uranium from 39.5% P2O5 industrial greed phosphoric acid
to determine the activity of the synthetic solvent to extract uranium from the P2O5 industrial greed phosphoric acid as source of uranium to determine is used .
Effect of aqueous /organic phase ratio on the extraction process
Different aqueous to organic phase ratio namely 1/1,1/2,1/3,2/1,3/1 and 4/1 were used to get the optimum phase ratio to remove high percentage
Effect of temperature on extraction process
The effect of temperature on the distribution coefficient reflects it results on the percentage of uranium extraction
Effect of mixing time on the extraction process
The effect of the mixing time or (contact time) on the extraction process was investigated.
Effect of settling time on extraction process
The effect of settling time on the extraction process was investigated .The extraction was carried out at optimum previously determined values and at room temperature.
Reextraction of uranium from the organic compounds
A stock solution of five litters solution is obtained used the previously determined factor for extraction then re-extraction process is carried out different reagents are used on the stripping of uranium from the organic material.
Precipitation of uranium from the strip solution
The strip solution containing uranium was precipitated using hydrogen peroxide as an efficient selective precipitating agent.