VOLUME 4, NO2, JUN 1982
12
 
Mass Spectra of NN-Linked Bi(pyridones) and Their Isomeric Pyrans

A S AFRIDI ,

A mass spectral fragmentation study for a number of NN-linked bi(pyridones) (V-VIII) has been carried out. The effect of substituents at the 2-, 4- and 6-position for these heterocycles have been investigated. The isomeric structures. VIII and IX might reasonably be exp"~ted to exhibit i.r: and n.m.r. spectra bearing some similarity to each other. The differentiation between the isomeric structures VIII and IX was achieved by mass spectrometry. Whereas the molecular ions (M'+) give frag­ment ions (M'+ -CO) due to the loss oftheC=O groups at the 2-and4-positions, daughter iOlls R-C=N'+ and R-O=O+ are obtained for 6-substituted pyridones and pyrans respectively. 
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Computer Genrated Monolayer Capacities and SpeciilC Surface Areas of Charcoal Using Organic Vapours as Absorbates

M SALEEM ,J AHMED ,M AFZAL ,

Computer generated monolayer capacity values and surface area values are reported for fourteen different compounds, adsorbed on charcoal. These values are obtained using Langmuir, Joyner, Kaganer and Reciprocal-pressure-volume equations on a IBM 360/G44 Computer programme. Our surface area and monolayer capaicty values differ from the well known BET values; an explana­tion for which is given.
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Chromatography on Hydroxylapatite and Electrophoresis in Polyacrylamide Gel of Protein Fractions from Lentil Seeds

S H SIDDIQUI ,

Total salt-soluble protein extract of lentil seeds was fractionated with differenct concentration intervals of ammonium sulphate. Fractions were separated by chromatography on hy­droxylapatite column. Chromatographic fractions were analysed by electrophoresis on polyacrylamide gel.The seeds contained a highly heterogeneous system of individual proteins. Fraction 0-30 was composed of minor protein components and nucleic acids. Fraction 30-60 was represented by primary and secondary globulins. The fraction which preciptated with ammonium sulphate of above 60% con­centration was dominated by vicilin and legumin. Which were inseparable on hydroxylapatite column and had maximum elution at 0.29 M phosphate buffer.
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The Dehydration Sequence of Nickel-Exchanged A Zeolites

S AKBAR ,

Five nickel (II) A - Zealites (16.6 -76.6% exchanged) were investigated using volu­metric, gravimetric, spectroscopic and magnetic susceptibility techniques. Upto 65% exchenged the fo~owing vacuum dehdtation sequence was determined:Ni+(H20)6 (Octahedral) 340K Ni2+(H20)3 (Ox)3  (quasi octahedral) 400K Ni2+(H20)2 (O2)3 (Trigonal bipyramid) 620K Ni2+ (O2)3 (Trigonal)(Where (Ox) represents the oxygen atom of the lattice of the zeolite).All the zeolites except 77% exchanged, showed the retension of the aluminositcate framework structures ~oth after preparation and upto 620K evacuation.
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Mixed Ligand complexes•of Zinc (ll) withNTA, EDTA and HEDTA as primary Ligands and Glutamic acid as secondary Ligand

A K SAXENA ,

Formation of mixed ligand complexes of Zn(I1) with NTA, EDTA and HEDTA as primuy ligands and glutamic acid as a secondary ligand has been studied potentiometrically. The -KMLA values are larger than K l:' and K2 values of simple Zn(II) - glutamate chelates. Further the stability sequence with respect to primuy Ugands is EDT A > HEDT A > NT A.
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Derivatives of 4-Hydroxy-6-Methyl-Pryan-2-one (Triacetic Lactone)

Zeeshan Shah ,

Acylation, using aliphatic dicarboxylic acid chlorides of triacetic lactone (1) has led to the formation of bispyran-2~nes of type (10. The bispyrones (Ila) and (lIb) on treatment with hydrochloric acid gave bispyran-4~nes (IVa) and (IVb) respectively. The action of methyl amine on (lIa,b) yielded the corresponding bispyridones (Va,b). Reactions of (1) with other electrophiIic reagents such as thionyl cWoride, Vilsmeyer formylation mixture (dimethyl formamide and phosphor­yl cWoride) and benzene diazonium chloride have resulted in the formation of (VIla), (VIlla) and (VlIIb) respectively. 3-Amino-derivatives (VlIId) and (VIlle) have also been prepared. The 3-position of (1) has been found out to be the exclusive site of electrophilic substitution reactions. The spectro­scopic data of the compounds has also been recorded.
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Electronic Spectra of Amminenickel (II) Halides and Psedohalides

D M S MOSHA ,

Ligand field splitting parameters (IOD9) for the complexes Ni(NH3)2O2 (X=Br,I., NCS; n=6,4,2) have been obtained from electronic specta. The use of these results for the calcula­tion of additional lODq values for NiBr2, Nil2 and Ni(NCS)2 or [Ni(NCS)6]4. is discussed. There is reasonable agreement between experimental and calculated values. A spectrochemical series for the ligands is presented.
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A New Synthesis of B-Carbolines by Metal Ion-Caltalysed Reaction Reduction of N-Imidotryptamines

A U RAHMAN ,A A ANSARI ,N SULTANA ,M GHAZALA ,M BASHIR ,

A New Synthesis of B-Carbolines by Metal Ion-Caltalysed Reaction Reduction of N-Imidotryptamines
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Preparation and thennal alicUYus of 1,4-0xathian Complexes of Silver(I) perchlorate and Copper(I) perchlorate. CryBtalBtructures of perchlorato-l,4-oxathian silver(I), perchloratiobis-(1,4-oxathian) silver(I) and tetrakis (1,4-oxathian) copper(I) perchlor

J D PATON ,J C BARNES ,C S BLYTH ,

The new compounds AgClO4 tx(lIl), AgCI04. 2tx(lV) and CuC104. 4tx (V) are reported. On heating, III and AgClO 4 3tx(I) explode without previous decomposition. IV and V also explode after partial loss of oxathian(tx). CuCIO 4' 3tx(lI) decomposes in two steps to CuCI without explosion. The crystal structures of III, IV and V havc been determined.III Orthorhombic Pea21, a = 9.597(5), b= 6.369(6), c= i3.643(4)A. Z'"4. R=0.080 for 836 rc­flexions. The structure is polymeric with square pyramidal coordination at the silver atom. Ag-S = 2.59 A, Ag-Q = 2.47 - 2.67 A. IV Monoclinic P21, a = 6.62(1), b = 16.80(2), c = 6.34(2) A, C'" 94.5°, z =2. R = 0.073 for 1303 reflexions. The structure is trigonal monomeric, with Ag-g = 2.44 A, Ag-Q = 2.62 A, S-Ag-S = 160.3°.V Monoclinic P21/n, a = 18.47(2), b = 7.75(1), c = 17.64(2) A, c = 92 5°, Z= 4. R = 0.097 for 1433 reflexions. The structure contains tetrahedral Cu (tx) 4+ cations Cu-S = 8.32 A. 
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Possible Antifertility Compounds - Part IV: Syntheses of 2-(Phthalimido methylamino)¬substituted benzanilides

A UPRETI ,S S TIWARI ,R K SATSANGI ,

Few benzanilides were synthesised by the condensation of· N-Phthalimido-antluanilic acid chloride with several amines. The compounds tested did not show anY post-coital effect for male fertility, and no antiimplantation activity was exhibited for female fertility.
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