VOLUME 9, NO2, JUN 1987
12
 
SYNTHESIS AND STRUCTURE OF DL-CAMPHOR-10-SULPHONANILIDE AND THE N-METHYLTHIADIZINEDIOXIDE

W JONES ,C R THEOCHARIS ,L WU ,R J CREMLYN ,

Camphor-10-sulphonanilide (3) has been prepared and the structure confirmed by X-ray crystallography. Comphor-10-sulphonyl chloride reacts with N-methylhydrazine to give the N-methylthiadiazine dioxide (4) and not the expected N-methylhydrazide (6). The reasons for this reaction are discussed. The structure of (4) was confirmed by X-ray analysis; the structures (3) and (40 were also supported by 1H and 13C-NMR spectroscopy.
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REACTION OF 3-CARBETHOXY-5,6-BENZOCOUMARIN WITH ANTHRANILIC ACID AND SYNTHESIS & SOME REACTIONS OF 3(3',1'-BENZOXAZIN-4'-ONE)-5,6-BENZOCOUMARIN

M A.I SALEM ,M A EL-KASABY ,

Treatment of 3-carbethoxy5,6-benzocoumarin (1a) with anthranilic acid gives 4-anthramiloyl-3-carbethoxy-3,4-dihydro-5,6-benzocoumarin (11a) and 3-carbethoxy-3,4-dihydro-5,6-benzocoumarin (IIIa) was synthesized also. Alkaline hydrolysis of (IIIb). On the otherhand the action of anthranilic acid on (1a) at 170oC gave (IIIc). (IIIa) and (Id). Cyclization of (Id) by acetic anhydride occurred and (IV) was obtained. Acidic or basic hydrolysis of (IV) gave the same product (Ic). While ammonolysis of (IV) gave (Ie). The behaviour of both (delta)-lactone and oxazinone rings in (IV) towards different amimes, hydrazines wre studied and aromatic hydrocarbons under Friedel-Crafts comditions.
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BEHAVIOUR OF 1'-HYDROXY-3(p-METHOXYPHENYL)-2'-ACRYLONAPHTHONE TOWARDS SOME NUCLEOPHILIC AND ELECTROPHILIC REAGENTS

E A SOLIMAN ,E M RAGAB ,A N REDWAN ,

Michael condensation of 1'-hydroxy-3-(p-methoxyphenyl)-2-acrylonaphthone (1) with acetylacetone and ethyl acetoacetate gave the cyclohexenone derivatives (IIa and b). Compound (I) reacts with paraformaldehyde in amyl alcohol to give (III) which condensed with acetylacetone to give (IV). Reaction of (I) and (IIa) with ethyl chloroacetate and ethyl iodide gave (XIII) and (XVII). The action of hydrazines, hydroxylamine hydrochloride, wrea, thiourea and amines on the above products has been described. 
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ELECTRONIC SPECTRA STUDY OF BARBITURIC AND THIOBARBITURIC ACID WITH MOLECULAR ORBITAL CALCULATIONS

A M HEIBA ,M S MASOUD ,A A HASANEIN ,

The electronic spectra of barbituric acid (BA) and thiobarbituric acid (TBA) in different solvents have been analyzed using the multiple linear regression technique to relate the shift in peak locations to some solvent polarity parameters. The PPP method has been used to study the tautomerism and calculate the different singlet-singlet electronic transitions in these molecules. 
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ISOLATION OF HIGHLY ACTIVE PAPAIN FROM DRIED PAPAYA LATEX

ZULFAQAR ALAM KHAN ,AHMAD SAEED ,IKRAM ULLAH KHAN ,

Papain, the cysteine proteinase, from dried papaya latex was purified by ammonium sulphate fractionation followed by agarose mercurial chromatography. The enzyme was further purified by covalent chromatography on thiol-Sepharose column in order to obtain 95-100% pure form. The purified enzyme was homogeneous on polyacrylamide gel electrophoresis with or without sodium dodecyl sulphate. The enzyme had a molecular weight of 23, 400 as determined by SDS-polyacrylamide gel electrophoresis. He reactions with 2,2'-dipyridyl disulphide and dithiobisnitrobenzoic acid showed that highly active papain contains one-SH group per enzyme molecule.
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SYNTHESIS AND CHARACTERIZATION OF PLATINUM (II) AND PALLADIUM (II) COMPLEXES WITH 2,5-DIMETHYL-4-HYDROXYPRIMIDINE

R P RAVAL ,A ADEYEMO ,

The binding of Pt(II) and Pd(II) ion 4-amino-2,5-dimethyl-1-pyrimidine (ADMPY) has been compared with the binding of the same metal ions to 2,5-dimethyl-4-hydroxy pyrimidine (HDMPY), analogue of ADMPY in which the amino group has been replaced by a hydroxyl group. A brief comparison is made with the corresponding Pt(II) and Pd(II) complexes of thiamine and oxythiamine. In this paper we report the synthesis, elemental analyses, infrared spectra data, proton and carbon-13 nuclear magnetic resonance studies of these new complexes. A complete assignment of 1H 13C NMR spectra resonances is presented for both the ligand and the complexes. The results show that the metallation site is N-1' position of the ligand in agreement with earlier works [1-3], however, the chemical shifts observed for this ligand upon complexation are larger than the corresponding chemical shifts observed for the 4-amino-2,5-dimethyl-pyrimidine analogue contrary to the thiamine/oxythiamine system. 
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CHELATING BEHAVIOUR OF SUBSTITUTED 3-ARYLHYDRAZOPENTAN-2,4-DIONE (PART X) STRUCTURE OF COPPER (II) COMPLEXES OF 2-METHOXY, 2-CHLORO, 2-BROMO AND 4-FLUOROPHENYLHYDRAZOPENTAN-2,4-DIONE

B A SHETARY ,M S ABDEL-MOEZ ,

Infra-red and U.V. visible spectra studies were carried out on copper (II) complexes of 2-methoxy phenylhydrazoacetylacetone (2-MeOPHA), 2-chlorophenylhydrazoacetylacetone (2-C1-PHA), 2-Bromophenylhydrazoacetyl-acetone (2-BR PHA), and 4-fluorophenylhydrazoacetylacetone (4-FPHA) organic ligands. The composition of complexes was found to be 1:2 (metal to ligand) stoichiometry and the structure of complexes was proposed to be square planar. The proton-ligand dissociation constant (pK) and the stability constants (log K1 and log K2) of their copper complexes have been determined pH-metrically at 30oC and at ionic strength 0.1 in 75% dioxane-water medium. The stability constants was found to be in the following order.
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BEHAVIOUR OF 3-NITROBENZAL-P-ISOPROPYL OR P-CHLORO-ACETOPHENONES TOWARD OVYGEN AND CARBON NUCLEOPHILES AND SOME STUDIES WITH THE PRODUCTS

M A SAYED ,N MOSTAFA ,M EL-MOBAYED ,M A EL-HASHASH ,A F EL-FARARGY ,

3-Nitrobenzylidene-p-isopropylacetophenone (1a) reacts with hydrogen peroxide to give the oxirane derivative (2). The cleavage of the strained oxirane ring with oxygen nucleophiles e.g. OH or nitrogen nucleohpiles e.g.hydrazine hydrate or hydroxylamine has been described. The reaction of  (1) with ethylcyanoacetate in the presence of ammonium acetate leads to the formation of nicotinonitrile derivative (7) toward wome electrophiles e.g. ethylchloroacetate or dimethyl sulphate or  some nucleophiles e.g. phosphorous oxychloride has been investigated.
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OXIDATION OF SOME ORGANIC ACIDS USING SODIUM BISMUTHATE IN AQUEOUS AND ACIDIC MEDIA

G E.M MOUSSA ,A N HEGAZI ,M E SHABAN ,F A FOULI ,

 The study includes oxidation of lactic, citric, tartaric, malic, mandelic, (alpha)-hydroxy isobutyric and isobutyric acids by sodium bismuthate as an oxidizing agent. The oxidation reactions were carried out in water, aqueous sulphuric (1-> 4N) or glacial acetic acid, using different molar proportions of sodium bismuthate. A tentative mechanism of oxidation is given and discussed. 
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RING OPENING OF SOME FURAN DERIVATIVES BY NUCLEOPHILES

A I MONEER ,A MOHAMED EL-KASABY ,

(Alpha)-3-Arylidene-5-[2¢-(p-cymyl]-spirofuran-3(2H)-2-ones (1a-d) were reacted with primary amines and gave cinnamamide derivatives (1Va-h) which were cyclized by the action of acetic anhydride and yielded the desired pyrolin-5-ones (VA-h). also (1a,b) were reacted with aromatic amines and anthranilic acid, the products pyrolin-5-one derivatives (Vi-n) were obtained.Action of ethanolic hydrazine hydrate on (Ia-d), (II) and (IIIa,b) were investigated either at room temperature or in boiling ethanol. Sodium hydroxide was affected on (IVi-I) and gave (Vla-d) also (VII) was condensed with benzaldehyde and yielded (IX). Cyclization of (VII) and (X) were investigated. All the structures of the adducts were confirmed via either analytical data or spectroscopic possible tools. 
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