bluuebunny/crossref_metadata_2025 huggingface dataset:
Determination of Trace Iron(II) in the Presence of Iron(III)
Authors: Luo Chien‐Shu , Hwang Jon‐Mau , Pung Tong‐Chuin , Tsai Hui‐Tuh
Published: June 2015

The determination of trace iron(II) is usually interfered by the presence of iron(III) when ortho‐phenanthroline colorimetric method is used. In this report a chromogenic reagent which contains ortho‐phenanthroline‐EDTA mixture has been developed to decrease the interference of ferric ion after adjusting the acidity of sample at 0.1 N by adding the sulfuric acid.

The procedure is also simplified by introducing sulfamate buffer solution (pH= 1.5) without adjusting the acidity of sample with sulfuric acid. If iron(III) is not present in the sample, this method is also applicable. The comparative results are exhibited for the present method and the conventional o‐phenanthroline method.
Electrochemistry in Organic Synthesis.: I. Large‐Scale Preparation of Cysteine From Cystine
Authors: Wong Chi‐Huey , Wang Kung‐Tsung
Published: June 2015

Cysteine hydrochloride was prepared by electroreduction of cystine with stainless steel plate as electrodes. 0.25 M of cystine in 1.5 N HC1 as cathode solution was divided by anion‐exchange membrane from anode solution (1.5 N HC1). A current of 5.6 A/S was applied and at the end of reaction, crysteine hydrochloride was obtained by evaporation of the cathode solution. The method is more convenient than the existing method.
A New Numerical Method for Automated Spectral Isolation of Component Substances in a Set of Mixtures
Authors: Lin Chi‐Hsiung , Liu Shi‐Chung
Published: June 2015

A new numerical method for isolating component spectra from spectra of their mixtures is presented. The method searches the component spectra by optimizing a risk function which assigns a relative value for the risk to regard a spectral shape as that of a pure substance. No prior knowledge of the nature of existing components is required in the analysis. All components conceivable in the set of mixture spectra are simultaneously isolated.
Reactions of Oligomeric Difluorosilylenes with Cis ‐and Trans‐Difluoroethylene
Authors: Liu Chao‐Shiuan , Hwang Tsai‐Lih
Published: June 2015

The reactions of oligomeric difluorosilylenes with cis ‐and trans ‐difluoroethylene are studied. All six new products are characterized and the stereochemistry suggests an integrated reaction mechanism in which both addition and insertion pathways share a common diradical transition state.
Enzymatic Synthesis of Oligopeptide. Part I. Papain‐Catalyzed Synthesis of Dipeptide, Tripeptide and Tetrapeptide
Authors: Chou Shan‐Ho , Chen Shui‐Tien , Wong Chi‐Huey , Wang Kung‐Tsung
Published: June 2015

Eighteen Z‐X‐Y‐OTNB+ type dipeptides, four Z‐Val‐Cys(Bzl)‐X‐OTMB tripeptides and a tetrapeptide Z‐Val‐Cys(Bzl)‐Cys(Bzl)‐Asn‐OTMB have been synthesized by papain‐catalyzed reaction in reasonable yield after recystallization. Z‐DL‐Ala‐OH has been resolved through papain‐catalyzed synthesis of Z‐L‐Ala‐Leu‐OTMB with an optical purity as high as 98.6%. These results show that papain is a good catalyst for oligopeptide synthesis.
Characterization of the Phosphoryl‐Nitrogen Linkages in Histone H4
Authors: Bruegger B. B. , Delange R. J. , Smith R. A. , Lin Y. C.
Published: June 2015

In earlier work we nave described and partially characterized two histone kinases from regenerating rat liver and other tissues which catalyze the transfer of the γ‐phosphoryl group from ATP to histones. The histone phosphates thus formed were observed to be acid‐labile and base‐stable. In the present study we report on the specificity of one of these enzymes, namely, the kinase which is optimally active at pH 9. This enzyme appears to be relatively specific for the two histidine residues of histone H4. These histidines occur at positions 18 and 75, and both are phosphorylated. However, when regenerating rat liver was the source of enzyme, the product was 1‐phosphohistidine, whereas the enzyme from Walker‐256 carcinosarcoma catalyzed the formation of 3‐phosphohistidine.
Synthesis of 2‐(6‐Methoxy‐2‐Quinolyl) Chromone Derivatives
Authors: Hsu K. K. , Wu T. S.
Published: June 2015

In the continuous investigation of structure and activity correlation of flavonoids, several 2′‐hydroxy‐2‐6(6‐methoxy‐2‐quinolyl)chromone derivatives and their intermediates 2′‐hydroxy‐2‐(6‐methoxy‐2‐quinolyl)acrylophenones were synthesized by the condensation of 6‐methoxy‐2‐quinoline aldehyde with appropriate 2‐hydroxoxy‐acetophenones in the presence of alcoholic potassium hydroxide, and then oxidized by selenium dioxide.
Metal Chelate Complexes of the Schiff Bases Derived from Salicylaldehyde and Methyl Ethers of Aminophenols (Anisidines)
Authors: Dubey K. P. , Kachru C. N. , Wazir B. L.
Published: June 2015

Some transition metal chelates of the Schiff's bases derived from salicylaldehyde and o ‐anisidine, m ‐anisidine and p ‐anisidine have been isolated and characterized. The structures of these complexes have been discussed on the basis of their elemental analyses, conductivities, magnetic moment values, electronic and infrared spectral data.

The Ni2+, Cu2+ and Zn2+ form ML2 type compounds, UO22+ and Fe3+ form dimeric [UO2 L2]and [Fe L2 Cl]2 respectively.
Molecular Structure of 4‐(p‐N, N‐Dimethylaminostyryl) Pyridine Methiodide
Authors: Lu T. H. , Lee T. J. , Wong C. , Kuo K. T.
Published: June 2015

C18H19N2I, Mr=366.24, monoclinic, space group P21/n, a=6.298, b=7.659, c=32.579 Å,β=101.54° (from Syntex Pl̄ diffractometer), Z=4. Dc=1.59, Dx=1.58(2)gm cm−2 (by flotation), m. p. 253°C. The compound was solved primarily by heavy atom method. The final R value was 0.067.
The Extractive‐Spectrophotometric Determination of Iron(III) As a Mixed‐Ligand Complex with N‐Hydroxy‐N, N′DI‐p‐Tolyl‐p‐Toluamidine and Thiocyanate
Authors: Patel K. S. , Deb K. K. , Mishra R. K.
Published: June 2015

The extractive‐photometric determination or iron(III) as a mixed‐ligand complex with N ‐hydroxy‐N, N′ ‐di‐p ‐tolyl‐p ‐toluamidine (HDTTA) and thiocyanate is described. The orange‐red Waterinsoluble 1:1:2 (metal: HDTTA: SCN−) ternary complex formed in 0.1–0.6 M hydrochloric acid solutions is quantitatively extractable into benzene. The wavelength of maximum absorption, molar absorptivity and sensitivity of the colour system are 460nm, 12000 l. mole−1 cm−1 and 0.0046 μg Fe/cm 2respectively. The influence or foreign ions on the determination of iron has been studied. This method has also been applied to determine the iron content of several alloys.
Quantitative Estimation of Ruthenium(III) Using Morpholine‐4‐Carbodithioate as a New Analytical Reagent
Authors: Kumar Ravindra , Singh Nepal , Kansal B. D.
Published: June 2015

Ruthenium(III) has been precipitated gravimetrically in the pH range 7.0‐8.5 with morpholine‐4‐carbodithioate and determined by weighing as a black complex (C5H6ONS2)3 Ru after drying at l00–110°C. The interference of the various metal ions has been avoided by using an ammonical mixture of EDTA and tartrate (1:1 molar ratio). The complex is thermally stable up to l60°C.
Synthesis of Optically Active l‐Menthol Part II. Isolation of dl‐Menthol from the Mixture of dl‐Menthol Isomers
Authors: Chang Teh‐Chou
Published: June 2015

The mixture of dl ‐menthyl chloroaeetate isomers and the mixture of dl ‐menthyl cyanoacetate isomers were prepared by the esterification of the mixture of dl ‐menthol with chloroacetic acid and cyanoacetic acid, respectively. In these mixtures the dl ‐menthyl chloroacetate m. p. 23–24° and the dl ‐menthyl cyanoacetate m. p. 63–63.5° are crystal form, the other isomers, such as dl ‐isomenthyl cyanoacetate b.p. 136–138°/3mmHg are liquid form. The crystal form ester was isolatded from liquid form ester by cooling crystallization, and then dl ‐menthol m. p. 32–33° was obtained by hydrolysis. The isolation effect has intimately relation to the dl ‐menthol content in raw material, the more dl ‐menthol content, the more yield and purity of crystal form ester, therefore, after hydrolysis, the obtained dl ‐menthol was excellent in purity.
Study of the Extractive Constituents from the Wood of Cuninghamia Konishii Hayata
Authors: Cheng Yu‐Shia , Lin Cheng‐Shan
Published: June 2015

From the neutral fraction of the acetone extractive of the wood of Cuninghamia konishii Hayata, α‐terpineol, cedrol, α‐cedrene, β‐cedrene, caryophyllene, α‐terpinyl acetate, cedryl acetate, α‐terpineol oxide, caryophyllene oxide, docosanol, tetracosanol, hexacosanol, β‐sitosterol and stigmasterol were isolated. Straight chain saturated hydrocarbon (C20H42‐C30H62) were also obtained.
Spectral Studies of Mercaptoacid Amides III: Nuclear Magnetic Resonance Spectra
Authors: Bateja S. , Chandrashekhar S. , Bhandari C. S. , Sogani N. C.
Published: June 2015

NMR spectra of twelve newly synthesised mercaptoacid amides are being reported and discussed.

The syntheses and structure of more than thirty mercaptoacid amides have been reported(1‐3) from our laboratories. The study has revealed that N ‐phenyl‐2‐mercaptoacetamide and related compounds have intramolecular hydrogen bonded structure (I).

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Determination of Palladium Using Hydroxylamine Hydrochloride as Metal Precipitant
Authors: Raoot Sarala , Vaidya V. G.
Published: June 2015

An analytical investigation on the quantitative reduction of palladium (II) to the metal with hydroxylamine hydrochloride in alkaline medium has been carried out. Accurate and reproducible results for the gravimetric determination of 3 to 30 mg of palladium have been recorded. Effects of various foreign metal ions on the determination have been studied.
A Comparative Study of Chemical‐Initiated and Radiation‐Induced Graft Copolymerization of Methyl Methacrylate onto Bamboo by Infrared Spectroscopic Technique
Authors: Lin K. C. , Lin Y. S. , Hsu T. C.
Published: June 2015

Graft copolymerization of methyl methacrylate onto bamboo was evidenced by means of infrared spectroscopic technique. A comparative study of chemical initiated and radiation‐induced grafting methods was made. The chemical‐initiated copolymerization treatment with water as the swelling agent can yield high grafting percentage, whereeas the radiation‐induced copolymerization treatment gives very low grafting percentage.
Synthesis of Insect Sex Pheromones and Their Homologues I. (Z, E)‐9, 11‐Alkadienyl Acetates
Authors: Lin Yuh‐Meei , Chow Yien‐Shing , Hsu Stella C. L.
Published: June 2015

(Z, E)‐9, 11‐Tetradecadienyl‐l‐acetate (1), a major component of the sex pheromone of Spodoptera litura (F.), and (Z, E}‐9, 11‐pentadecadienyl‐1‐acetate (2) were synthesized by the Wittig reaction between (E)‐2‐alkenal (3) and the ylid derived from 9‐hydroxynonyltriphenylphosphonium bromide (4).
Kinetics of Silver‐Catalysed Oxidation of dl‐Atrolactic Acid (A. L. A.) by Potassium Peroxydisulphate
Authors: Singh Hambir , Prasad Mahesh , Saksena S. C. , Kansak B. D.
Published: June 2015

Kinetic data of silver catalysed oxidation of dl‐atrolactic acid (A. L. A.) by peroxydisulphate ion are reported. The reaction is first order with respect to S2O52 ion zero order with respect to A. L. A. The rate is linearly related with Ag+ ion concentration. The oxidation products of A. L. A. were found to be CO2and acetophenone, which establish the fission of C‐C bond in the oxidation process. The mechanism of the reaction and inhibition by various substrats has been discussed.
Lanthanon (III) Derivatives of Monofunctional Bidentate Schiff Bases
Authors: Gharia K. S. , Mathur (Miss) Shakuntala , Singh Megh , Sankhla B. S.
Published: June 2015

The 1:1, 1:2 and 1:3 interactions of lanthanon (III) isopropoxide with monofunctional bidentate Schiff bases as salicylidene‐o‐toluidine (SOTH) and salicylidene‐p‐p‐toluidine (SPTH) have been investigated. The resulting products Ln(OPr1)2(SB), Ln(OPr1)(SB)2 and Ln(SB)3 (where Ln=Pr, Nd and Sm and SB1− is the anion of the corresponding Schiff base) have been isolated in almost quantitative yields. The infrared spectra of these compounds have been recorded and plausible structures suggested.
A Sensitive Spectrophotometric Determination of Niobium (V) with 5, 7‐Dinitro‐8‐Hydroxyquinoline
Authors: Sharma Yogendu , Shivahare G. C.
Published: June 2015

Niobium (V) reacts with 5,7‐dinitro‐8‐hydroxyquinoline to form yellowish‐orange coloured complex having maximum absorbance at 420 nm in citric acid medium. The reaction is slow at room temperate, it is complete in 15 minutes at temperate 40°. The colour is stable for at least 16 hours. Effects of heating temperate, time, pH, reagent concentration and other variables have been studied. The system confirms the Beer's law over the concentration range investigated. Optimum condition range for measurement in 10 mm cell is 1–12 μg of niobium. The molar absorptivity is 5.327 × 108 litre moles−1cm−1. The interference from foreign ions has been evaluated. The metal ligand ratio of 1:2 was confirmed by Job's continous variation and mole ratio methods.
Assay of Aspirin, Ethenzamide and Caffeine Mixture by 13C NMR Spectrometry
Authors: Chiang Hung‐Cheh , Imanari Mamoru
Published: June 2015

13C FT NMR method of gated decoupling without NOE was applied in the quantitative analysis of aspirin, ethenzamide and caffeine mixture (antipyretic). Spectra were obtained in pyridine‐d5, containing anisole as an internal standard and chromium(III) acetylacetonate as a paramagnetic relaxation reagent, The results were generally satisfactory.
Contstituents of Formosan Folk Medicines X. Chemical Constituents of the Rhizoma of Onychium Contiguum (Wall.) Hope
Authors: Wu Tian‐Shung , Chen Ming‐Tyan , Kuoh Chang‐Sheng , Yang Jih‐Jen
Published: June 2015

Phytosterol mixture (campesterol, 15.3%; β‐sitosterol, 84.7%), sucrose and kaempferitrin were isolated from the ethanolic extracts of the rhizoma of Onychium contiguum (Wall.) Hope (Pteridaceae).
Preparation and Analytical Application of a New Chelating Ion Exchange Resin Containing Thioglycolic Acid
Authors: Liu Chuen‐Ying , Sun Peng‐Joung
Published: June 2015

Starting from copolymerization of acrylonitrile and divinylbenzene by emulsion polymerization technique, a macroporous, crosslinked polyacrylonitrile copolymer was synthesized. The nitrile groups on the copolymer resin were converted into carboxylic acid groups by hydrolysis with strong alkaline solution of sodium hydroxide to obtain the resin matrix with carboxylic acid groups. A new chelating ion exchange resin containing alkylthioglycolate was prepared by esterification of carboxylic acid groups on the resin matrix and thioglycolic acid with 1,6‐hexanediol as binding part. After studies of the basic characters, ion exchange ability, exchange rate and acidity of the medium, it was found that the new resin obtaind was highly selective for silver(I), mercury(II), gold(III) and bismuth(III) in acidic‐aqueous solution. Separation of these metal ions from each other and concentration of these metal ions from very dilute solution were studied by liquid chromatography using a short column of this new resin. The analytical applications of this new resin are reported.
Electronic Absorption Spectra of Substituted Phenols
Authors: Masoud Mamdouh S. , Ali G.Y.
Published: June 2015

The spectral properties of o‐aminophenol, catechol, o‐nitrophenol, pyrogallol, salicylic acid and gallic acid were investigated in different solvents. The behaviour of hydrogen bonding demonstrated in these systems was discussed.
Some Cyclopentadienyl and Indenyl Niobium(V) Phenoxides
Authors: Rastogi M. K. , Nigam S. N.
Published: June 2015

Some cyclopentadienyl and indenyl niobium(V) phenoxides are reported in this communication. The effect of different types of groups in the phenoxide ring is related with the stability of the compounds. It has been established that only those phenols which have two hydroxyl groups in the ortho position are able to form chelates. The cyclopentadienyl and the indenyl rings are π‐bonded to niobium atom. The complexes have been characterised by elemental analysis and i.r. spectra.
The Stabilities and Thermodynamic Properties of Thorium(IV) and Zirconium(IV) Chelates of Ethylenebis (Oxyethylenenitrilo) Tetraacetic Acid
Authors: Hseu Tong‐Ming , Jyi Kae‐Ming
Published: June 2015

The interaction between ethylenebis(oxyethylenenitrilo)tetraacetic acid (EGTA or H4Z) and Th(IV) and Zr(IV) ions has been investigated potentiometrically by using a mercury indicator electrode. The formation constants of the chelates ThZ and ZrZ have been evaluated at a constant ionic strength of 0.10 (KNO3) and at 0, 10, 20, 30 and 40°. Enthalpy and entropy changes characterizing the formation of the chelates have been calculated by the least‐squares method at 25°. The results are collected as follows:

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Spectrophotometric Determination of Copper with Diacetylmonoquinolylhydrazone
Authors: Anipindi A. R. , Jain P. , Singh R. P.
Published: June 2015

Synthesis of a new reagent diacetylmonoquinolylhydrazone (DAmQH) and its application in the selective spectrophotometric determination of copper is presented. DAmQH reacts with copper instantaneously to form a green complex in the pH range 7.5–11.6 with molar absorptivity 1.45 × 104 l mole−1 cm−1. Beer's law is obeyed upto 2.20 ppm of copper. Copper has also been analysed in several alloys.
Valence Charge Transfer in Cubic BN Crystal by X‐Ray Diffraction
Authors: Chen Ruey‐Hong
Published: June 2015

The X‐ray diffraction data of cubic BN were reanalyzed by aspherical electron charge distribution model. The valence‐charge densities of nitrogen atom and boron atom were represented by a finite multipole deformations. A least‐squares refinement of the model charge was computed by fitting population parameters and thermal parameters. The result showed that there is a tendency toward a ionic bond in going from IV‐IV compouds to III‐V compounds.
Application of Iodide Ion Selective Electrode to the Study of Stepwise Formation Constant and Solubility Product of Lead Iodide
Authors: Chang Wen‐Lie , Chang Fu‐Chung , Wu Shaw‐Chii
Published: June 2015

Iodide ion‐selective electrode were studied, prepared and applied for the complex formations and solubility product determination. The thermodynamic formation constant of PbI+ and the solubility product of PbI3 were found to be 54 and 9.2 × 10−9, respectively. The formation constant of PbNO3+ was calculated to be 4.6 from the different formation constant of PbI+ in perchlorate and nitrate media.
A Convenient Procedure for Phase Transfer Catalyzed Acetylation of Hindered Phenols
Authors: Liu Kwang‐Ting , Kuo Mann‐Yan
Published: June 2015

A facile and generally applicable procedure for acetylation of hindered phenols using tetra‐n‐butylammonium bromide as phase transfer catalyst and acetic anhydride as acetylation agent has been developed. The isolation yield is 85–91%.
Preparation and Characterisation of Bis (η5‐Cyclopentadienyl) N,N‐Disubstituted Dithiocarbamato Chloro Oxotungsten (VI) Complexes
Authors: Kaushik Narender K. , Sodhi Gurvinder S. , Sangari Harpal S. , Chhatwal Gurdeep R.
Published: June 2015

Bis (η5‐cyclopentaienyl) N,N‐disubstituted dithiocarbamato chloro oxotungsten (VI) complexes of the type η5‐Cp2WO(S2CNR2)Cl and η5‐Cp2WO(S2CNRR')Cl (where R=Me, Et and i‐Pr and R'=Cyhx) have been prepared by the reaction of bis (η5‐cyclopentadienyl) oxotungsten (VI) dichloride with sodium salts of dithiocarbamic acids in refluxing tetrahydrofuran. Infrared spectral studies demonstrate that in these complexes dithiocarbamate ligands are bidentate. Therefore, tungsten (VI) atom may be assigned a coordination number 6 in all these complexes. Elemental analyses of these compounds have also been carried out. Electronic spectra have been recorded for all the six complexes.
Regiospecific Syntheses of Sulfoxides and Sulfones of the (Z)‐Configuration
Authors: Liu Lilian Kao , Luo Fen‐Tair , Shia See‐Ying
Published: June 2015

A convenient synthesis for varions (Z)‐1‐alkanesulfinyl‐2‐phenylethenes has been developed. This involves addition of different sodium thiolates to phenylacetylene in ethanol, and oxidation of the resulting (Z)‐1‐alkanesulfenyl‐2‐phenylethenes [(Z)‐styryl alkyl thioethers] with sodium metaperiodate supported on acidic alumina. The corresponding sulfones can be obtained by oxidation of these (Z)‐styryl alkyl thioethers with hydrogen peroxide in glycial acetic acid, or, alternatively by reduction of the β‐iodostyrylsulfones with zinc in acetic acid. These β‐iodostyrylsulfones were obtained by addition of the corresponding sulfonyl iodides to phenylacetylene under the catalytic action of cupric chloride and triethylaminium chloride.
The Complexation of Lanthanides by AZO‐β‐Diketones Stability Constants
Authors: Zahra A.M. , Ramadan A.A.I. , El‐Shetary B.A. , Abdel‐Moez M.S.
Published: June 2015

The stability constants of the complexes between the trivalent lanthanide series of cations and series of azo‐β‐diketone ligands are reported. The measurements were conducted at 30° at an ionic strength of zero, in 100% methanol.

The relation between the overall stability constant (log β2) and atomic number of the lanthanide elements, shows a buffer zone at the gadolinium area. The relation between (log β2) and the basicity of the studied ligands (ΣpK's) are also, discussed.

The overall stability values obtained reflected a great affinity of the organic ligands for chelation with lanthanide ions.
The Study of Steric Effect on the Magnetic Interaction between Two Metal Ions in a Binuclear Complex
Authors: Wang Wen‐Jwu
Published: June 2015

Complexes of cupric ion with N,N′‐bis(2‐pyridylethyl)‐oxamide, prepared from 2‐(aminoethyl)pyridine and diethyloxalate, and pyridine derivatives have been synthesized and characterized by elementary analysis, i.r. spectra, u.v. spectra, magnetic susceptibility, and electric conductivity measurements. Existance of magnetic interaction between cupric ion could be recognized. Magnetic interaction may be affected by the pyridine derivatives.
Studies on the Ion‐Exchange Chromatographic Separation of L‐Ascorbic Acid and Oxalic Acid
Authors: Chang E.E. , Hsu Tong‐Jung , Kao W.Y. , Yang C.C.
Published: June 2015

L‐Ascorbic acid and oxalic acid could be successfully separated with a column of 8% cross‐linked sulfonated polystyrene cation‐exchange resin in hydrogen form, and eluted with 0.01% aqueous solution of nitric acid, sulfuric acid, or phosphoric acid. Among the mineral acids used, nitric acid showed the best separatory effect. The minimum detectable quantities of the acids were 0.05 μg and 0.5 μg per 0.5 ml sample solution for L‐ascorbic acid and oxalic acid, respectively. Under this condition, the acids could be detected by using automatic UV‐monitor apparatus.
Pyrolysis of Nickel Zirconyl Oxalate
Authors: Reddy V.B. , Mehrotra P.N.
Published: June 2015

Nickel zirconyl oxalate hexahydrate (NiZrOx) is δ prepared and characterised by I.R. spectral and chemical analysis. Its thermal decomposition has been investigated by employing TG, DTG, DTA and chemical analysis. End product was identified by X‐ray diffraction studies. The decomposition proceeds through four steps i) dehydration of NiZrOx in two steps, ii) partial decomposition of oxalate to give an oxalate carbonate intermediate, iii) decomposition of oxalate to give a non‐stoichiometric carbonate and iv) decomposition of this non‐stoichiometric carbonate to give the end product a mixture of NiO+ZrO2. On the basis of the results obtained, a tentative scheme for the decomposition of NiZrOx is proposed.
Decomposition of Triethylamine Over Acid Catalysts
Authors: Ebeid Fikry M. , Gheit Ahmed K. Aboul , Ezzo Esam M. , Ali Leila I.
Published: June 2015

The effect of hydrochloric acid, boric acid, and silica content in alumina on its catalytic activity towards the decomposition of triethylamine was investigated at 310°, 320°, and 330°. The study was carried out in a flow system and the reaction product was analyzed chromotographically. Ethylene formation is a zero order reaction independent of the partial pressure of triethylamine. Treating γ‐alumina with hydrochloric acid increases its catalytic activity towards ethylene formation whereas silica‐alumina is less active than γ‐alumina. Boric acid‐treated alumina has the same activity of γ‐alumina. Formation of ethylene from preadsorbed triethylamine was studied. The similarity between reactions of aliphatic alcohols and amines over acid catalysts is concluded.
Spectrophotometric Determination of Cobalt(II), Nickel(II) and Copper(II) with Acenaphthenequinone Monosemicarbazone (AQSC)
Authors: Singh S.K. , Sindhwani (Miss) Kamini , Sindhwani S.K.
Published: June 2015

Cobalt(II), nickel(II) and copper(II) complexation with acenaphthenequinone monosemicarbazone (AQSC) has been studied spectrophotometrically. The Co(II), Ni(II) and Cu(II) complexes are soluble in ethanol medium and exhibit maximum absorbance at 410, 420 and 430 nm, respectively. The sensitivity of the reactions are 0.012, 0.02 and 0.01 μg/cm2 for cobalt, nickel and copper systems. All the three complexes show maximum and constant absorbance in the pH range 8.4 to 9.8, 6.3 to 8.4 and 5.4 to 8.0 for Co‐AQSC, Ni‐AQSC and Cu‐AQSC, respectively. Nickel and copper in some alloys have also been analysed.
Synthesis and Infrared Spectral Study of Neodymium Furfuroxides and Tetrahydrofurfuroxides
Authors: Solanki Ashok K. , Wadhwa Sarita , Bhandari Akshya M.
Published: June 2015

Nd(OR')3, Nd(OR)(OR')2 and Nd(OR)2(OR') are prepared from neodymium isopropoxide and furfurylalcohol and tetrahydrofurfuryl alcohol in different stoichiometric ratios under reflux where OR=OPri or OBu'; OR'=deprotonated furfuryl and tetrahydrofurfuryl alcohol. Neodymium tertiary butoxide derivatives were prepared by alcohol exchange technique from the corresponding isopropoxide derivatives. The i.r. spectra of the alkoxy derivatives are discussed.
Synthesis of Hexa‐O‐Methyl‐8‐(8“‐Naringeninyl)Apigenin
Authors: Lee Ing‐Huei , Chen Fa‐Ching , Lin Yuh‐Meei
Published: June 2015

The title compound was prepared from 8‐iodo‐5,7,4′‐trimethoxyflavone and 8‐iodo‐5,7,4′‐trimethoxyflavanone using modified condition for the Ullmann condensation.
Selective Spectrophotometric Determination of Copper in Milk with Phenanthraquinone Monothiosemicarbazone
Authors: Sinha P. P. , Kamil F. , Sindhwani S. K. , Singh R. P.
Published: June 2015

The red complex formed by copper (II) and phenanthraquinone monothiosemicarbazone has an absorption maximum at 530 nm with a molar absorptivity of 14000 cm−1 mole−1. The pH range for the determination is 1.1–6.6. Optimum range of concentration for accurate determination is 0.50–3.47 ppm of copper (II) in 50% methanol medium. The limits of interference due to foreign ions have been studied. The method has been successfully employed for the determination of copper in various samples of milk.
Preliminary Study on Indirect Polymerization with Electrolytically‐Generated Redox Initiators—A New Method of Polymerization
Authors: Lin Tzu Fang , Chung Jiann‐Sheng
Published: June 2015

FeCl3, CrCl3, CH3NH2·HCl and H3NNH2·2HCl were used as the electrolytes which were dissolved in water, methanol or DMF. The redox initiators which composed of oxidizing agent and reducing agent were produced in the anode and cathode chamber respectively through electrolysis. It was found that the redox initiators obtained by using organic electrolytes of CH3NH2·HCl and H2NNH2·2HCl have much better polymerization yield of MMA than those of using inorganic electrolytes such as CrCl3, FeCl3. The reasons of different yields with different electrolytes are also discussed.
Spectrophotometric Determination of Iron (III) Using 3‐Hydroxy‐2‐Methyl‐1,4‐Naphthoquinone Monoxime (HMNQM)
Authors: Kamini (Miss) , Kamil F. , Sindhwani S. K.
Published: June 2015

Iron (III) forms brown coloured complex with 3‐hydroxy‐2‐methyl‐1,4‐naphthoquinone monoxime. The iron (III)‐HMNQM complex is found to be soluble in DMF and exhibits maximum absorption at 470 nm in the pH range 4.5–5.5. Beer's law is obeyed upto 5.58 ppm of iron (III) and sensitivity of the reaction is 0.0046 μg/cm2, with molar absorptivity of 1.21×104 ℓ mole−1 cm−1. The method has been used for the determination of iron (III) in alloys.
Spectrophotometric and Polarographic Studies of the Uranium in Acetate Medium in the Presence of Resorcinol
Authors: Zahra Ahmed M. , El‐Inany Gaber A. , El‐Maraghy S. B.
Published: June 2015

Uranyl ion reduction was studied in acetate buffer‐resorcinol medium. Two waves were obtained for all pH. Resorcinol can be used as a maximum suppressor. Complexation of uranium with resorcinol was accompanied by a decrease in diffusion current and shift of half‐wave potential to more negative values. Mixed complexes of acetate and resorcinol were formed with uranium. Resorcinol stabilizes the pentavalent uranium by complexaion.
Polarographic Behaviour of Quinalidic Acid in Aqueous and Nonaqueous Solutions
Authors: Hindawey A. M. , Abou Ali S. A. , Salem T. M. , Mohamed G. B.
Published: June 2015

The polarographic behaviour of quinaldic acid is studied in aqueous universal buffer solutions as well as in mixed organic solvent viz. methanol, n‐propanol, dimethyl formanide (DMF) and dimethyl sulphoxide (DMSO).

The solvent proportion in the medium is maintained at 30% (v/v). The polarographic reduction gives two irreversible reduction waves. The nature of the waves and the electrode reaction are investigated. The electroreduction waves is proposed.
The Complexation of Some Transition Metals by Acetoacetanilidehydrazo Ligands “Stability Constants”
Authors: Taha Atef A. , El‐Inany Gaber A.
Published: June 2015

Acid dissociation constants of acetoacetanilide abbreviated (AAA); Orthocarboxy‐phenylhydrazoacetoacetanilide (o‐CPHAAA); and orthocarboxy‐phenylhydrazo‐parachloro‐acetoacetanilide (o‐CPH‐p‐Cl‐AAA) and chelate stability constants of the corresponding anions with Cu+2, Ni+2, CO+2, Zn+2, Mn+2, and Cd+2 ions are reported. The infra‐red spectra of o‐CPHAAA and o‐CPH‐p‐Cl‐AAA ligands and their chelates for copper and nickel are discussed.
Stability Of 2‐Carboxyphenylhydrazoacetoacetanilide, and 2‐Carboxyphenylhydrazobenzoylacetone Complexes of Rare‐Earth Elements in Mixed Solvents
Authors: Taha Atef A. , El‐Inany Gaber A.
Published: June 2015

The overall stability constants of the 1:1 and 2:1 2‐Carboxyphenylhydrazoacetoacetanilide (2‐CPHAAA) and 2‐Carboxyphenylhydrazobenzoylacetone (2‐CPHBA) rare‐earth chelates, were determined by a potentiometric method. The variation of the overall stability constants, “log β” with atomic number, of the lanthanide was ascribed to different degrees of dehydration of the cations. The 2‐CPHBA ligand exhibited less affinity for rare earth cations than 2‐CPHAAA.

The correlation of “log β” versus the basicity of the ligands showed that 2‐CPHAAA and 2‐CPHBA form the same type of chelate in polar solvents but differ in non polar solvents.
Catalytic Pyrolysis of Methane
Authors: Fang Treliant , Yeh Chuin‐Tih
Published: June 2015

Methane decomposition over metal oxides/SiO2 surface was investigated. At 1400 K obtained product distribution of this decomposition varied with metal oxide used. The effectiveness of these catalysts has been discussed in terms of activity and C2 selectivity. ThO2/SiO2 was found to be the most effective catalyst for the catalytic decomposition of methane. Positive catalytic effect of ThO2/SiO2 on the pyrolysis has also been confirmed at 1073 K. At low reaction conversions, ethane and ethylene are found as major products. Yields of ethylene and other unsaturated products are sensitively inhibited by NO impurities in the methane. A reaction mechanism has been proposed to account observed experimental results.
Compositions of the Essential Oils of Litsea Kostermanin Chang, Litsea Gerciae Vidal and Litsea Cubeba (Lour.) Persoon
Authors: Cheng Ming‐Chu , Cheng Yu‐Shia
Published: June 2015

The essential oils from the leaves and stems of Litsea kostermanin Chang and Litsea cubeba (lour.) Persoon, and the leaves of Litsea gerciae Vidal were analysed to determine the detailed composition of each oils. The major constituents were isolated and identified by GLC, IR, and NMR. The analyses showed that large chemical differences exist among L. kostermanin Chang, L. gerciae Vidal and L. cubeba (lour.) Persoon.
Cesium Ion‐Selective Electrode
Authors: Chang Fu‐Chung , Wu Shaw‐Chii , Huang Chiang‐Ho
Published: June 2015

The membrane material was prepared by mixing 40% of cesium‐triphenyl‐cyanoborate and 60% of PVC powder. The mixture was pressed at a pressure of 20tons/cm2 for 1hours to make the membrane. Then, the membrane was mounted on a self‐constructed electrode body. Nernstian slope of 60 mv/decade was obtained throughout the concentration range 10−1∼2×10−5M. Selectivity coefficients were presented. The life time of the electrode is longer than 6 months.
Gas‐Liquid Chromatographic Determination of Pipemidic Acid
Authors: Chen Su‐Hwei , Wu Hsin‐Lung , Lin Shun‐Jin
Published: June 2015

A gas chromatographic method was established for the quantitative analysis of pipemidic acid. The method is based on alkylation of pipemidic acid with diazomethane catalyzed by boron trifluoride. The sample was chromatographed on a stainless steel column packed with 5% OV‐101 on Chromosorb G‐HP and n‐octacosane was used as an internal standard. Quantitation is achieved by measuring peak‐height ratio. The method was satisfactorily applied to the analysis of pipemidic acid in tablet.
Synthesis of Some N‐Substituted Benzene Alkamines
Authors: Kachroo P. L. , Andotra Charanjit Singh , Langer T. C.
Published: June 2015

Synthesis of N‐β‐phenylethyl‐2:4‐dialkoxy‐5‐alkylbenzylamines having different alkyl and alkoxy groups have been described.
Differential Pulse Polarographic Determination of Trace Molybdenum in Uranium with α‐Benzoinoxime Extraction
Authors: Wu Cheng‐I , Chang Fu‐Chung , Yeh Yu‐Chai
Published: June 2015

A method for the determination of trace molybdenum in uranium is described based on its specific catalytic reduction wave in the presence of nitric acid. Molybdenum is separated from uranium by α‐benzoin oxime extraction and determined by differential pulse polarography. As lower as 1 ng/ml of Mo(VI) is determinable and 98% of recovery can be obtained at present work.
The Chemical Constitutents of Coniogramme Japonica (Thunb.) Diels
Authors: Chen Yu‐Min , Chang Teh‐Chou
Published: June 2015

β‐Sitosterol, β‐sitosteryl palmitate, β‐sitosteryl‐β‐D‐glucoside and cyclolaudenol were isolated from the rhizomes, long chain aliphatic esters and an UV stabilizer, octabenzone, were isolated from the leaves of Coniogramme japonica.
Molecular and Crystal Structure of Magnolol—C18H18O2
Authors: Wang Yu , Cheng Ming‐Chu , Lee Ju‐Shiung , Chen Fa‐Ching
Published: June 2015

Magnolol, 2, 2′‐dihydroxy‐5, 5′‐diallylbiphenyl (C18H18O2) was isolated from the heartwood of Taiwan sassafras, Sassafras randaiense (Hay.) Rehd. (Lauraceae) and characterized by single crystal X‐ray diffraction. It crystallized in monoclinic P 21/C. The cell parameters are a=10.905(3), b=8.834(4), c=16.103(9) Å, β=106.76°(3), z=4. The structure was solved by direct method. The dihedral angle between two benzene rings is about 45′ which seems to be the best arrangement for intra‐ and inter‐molecular H‐bondings. O … O distances are ∼2.6 Å which indicate very strong H‐bonding. The solid structure can be discribed as a helix chain of molecules connected through H‐bonds parallel to b‐axis.
The Photochemistry of Diazomethane‐Acetonitrile Mixtures. The Reaction of Methylene with Acetonitrile
Authors: Huang C. F. , Lin T. S. , Ho S. Y.
Published: June 2015

The photochemistry of diazomethane‐acetonitrile gaseous mixtures has been studied. Propionitrile was produced by the reaction of methylene radicals with acetonitrile. At lower pressures the product propionitrile decomposes and the measured decomposition rates are 1.14×109 sec−1 and 2.70×108 sec−1 at 3660 and 4358 Å, respectively.
Selective Separation of Gold on Amberlite xad‐4 Impregnated with Dmabr
Authors: Chien Chun‐Ching , Chang Fu‐Chung , Wu Shaw‐Chii
Published: June 2015

DMABR (5‐(4‐Dimethylaminobenzylidene)‐rhodanine) is proved to be a very selective reagent for gold as it impregnated on XAD‐4. Gold is selectively adsorbed on resin through the formation of Au(I)‐DMABR. Distribution coefficients at different pH were determined. The selectivity and interference were studied. Less than 0.1 ppb of Au could be adsorbed on resin. It can be directly determined by NAA or cluted down with cyanide solution and determined by AAS.
Average Configuration of Finite Polymer with Excluded Volume Interaction
Authors: Mou Chung Yuan
Published: June 2015

A quasi‐thermodynamic model for expansion of polymer configuration in solution is investigated. The model is based on Gaussian distribution of segments and mean field theory of polymer solution. An in‐homogeneous contribution to the free energy of solution is proposed. It arises from the nonhomogeneous distribution of polymer segements. This effects makes the expansion factor α to be larger than those without the effect considered. Some numerical consequence for the case Polydimethylsiloxane+cyclohexane solution is calculated. Our theory predicts a larger value a than the case without inhomogeneous effect being considered. The difference becomes less significant at higher molecular weight.
Mössbauer and Electrochemical Studies of Bridged Biferrocenes and Biferrocenylenes
Authors: Wei Ho‐Hsiang , Chang Shinn‐Jen
Published: June 2015

A series of neutral and oxidized π‐bridged biferrocenes (Fc—x—Fc) and biferrocenylenes (FC(—x—)2Fc) (x= —CH=CH—, —CH3,C=CCH3—) were prepared and their physical properties have been studied by means of Mössbauuer and cyclic voltammetry. The electrode reaction of these bridged ferrocene derivatives appears to involve a consecutive two‐step oxidation process. The results also show that the voltage difference between the first and second oxidaton potentials of the bridged biferrocenes was found to be largely exceeded that founded for the corresponding the bridged biferrocenylenes. The Mössbauer data show that the oxidation of doubly bridged Fc(—x—)2Fc with iodine, DDQ, and TCNQ given the corresponding dioxidized salts only and no stable mixed‐valence compounds were found.
Kinetics of the Reduction of Cupric Ion in Ammonia Solution by Sulfur Dioxide
Authors: Kao Chen‐Feng , Shih Yi‐Jen , Lai Tsai‐Teh
Published: June 2015

The reduction of cupric ion in ammonia solution by aqueous sulfur dioxide was studied. Each run was carried out at constant initial cupric concentration, stirred rate and total mixed gas flow rate. The effect of temperature, partial pressure of sulfur dioxide in gas phase and cupric ion concentration of the solution was investigated.

The reaction of Cu3++SO2(aq.)→Cu++SO42− was carried out by bubbling mixed gas (SO2/N2) through the aqueous ammonia complex of copper (II). The color change for the system was from deep blue, green, yellow to white. The pH values in the system changed from 10 to 4. The product of the reaction was identified by the analyses of IR spectrum and X‐ray diffraction, having the formula of 7Cu2SO3· 2CuSO3·3(NH4)2SO3·24H2O.

The kinetic model of the reduction was proposed as:

–d[Cu2+]/dt = k exp(–E/RT)[Cu2+]α[SO2%]

According to the experiments, the parameters were determined as:

α=1.64±0.03, þ=1.20, E=13.7 Kcal/mol and k = (1.77±0.20)×1010 (g‐equ./ℓ)−0.64min−2.
Studies of Orcein and Its Metal Complexes I. Spectral Behaviour of Orcein. Medium Effect and Ionisation Constants
Authors: Issa R.M. , Abu‐El‐Wafa S.M.
Published: June 2015

The electronic absorption spectrum of orcein is studied in organic solvent of varied polarities and water‐organic solvent mixtures with different pH. The absorption bands are assigned and the effect of solvent polarity on their position is discussed. The pka of the acid‐base equilibria set are determined and commented upon in relation to nature and proportion of the organic solvent added. The main bands of the ir spectrum and signals of the 1H nmr spectrum are as well discussed. The mixing of orcein with transition metal ions leads to drastic changes in colour and hence the visible absorption spectra of both organic compound and metal ions.
Coordination of Y(III), Ce(III), La(III) and Zr(IV) with Some Salicylidene Aromatic Schiff Bases
Authors: El‐Haty M. T. , Adam F. A. , Abdalla Nadia A.
Published: June 2015

Coordination compounds formed by the interaction of some salicylidene aromatic Schiff bases with Y(III), Ce(III), La(III), and Zr(IV) are prepared and characterized by elemental analysis, electronic and i.r. spectra as well as conductometric methods. The i.r. spectra indicate that coordination takes place through the azomethine nitrogen atoms and OH groups. The structure of such products depend mainly on the type of Schiff base used. Also, the formation constant of the complexes are evaluated.
A General and Improved Preparation of Monoketals of Symmetrical Diketones with Polymeric Protecting Reagent
Authors: Chou Ta‐Shue , Shih Yun‐Er
Published: June 2015

Monoprotection of symmetrical diketones could be accomplished by using polymeric supported 1,2‐diol by monoketalization of only one of the carbonyl groups. These monoprotected diketones could then undergo different types of reactions leading to selective synthesis on one ketone group only.
Some Aspects on Preconcentration for Neutron Activation Analysis
Authors: Yeh Si Jung , Lo Jem Mau , Wang E. L.
Published: June 2015

A preconcentration method incorporated with neutron activation analysis was developed for the accurate determination of trace metals in biological and environmental samples. Bismuth diethyldithiocarbamate, thallium diethyldithiocarbarnate, and ammonium pyrrolidinedithiocarbamate were used as the preconcentration agents for three groups of metals. Trace metals were enriched and interfering elements such as Na, Br, P. K. etc. were removed simultaneously during the preconcentration process so that the sensitivity for each metal was greatly improved. Optimal conditions for sample digestion, group preconcentration of trace metals and neutron activation analysis of biological and environmental samples were discussed.
Reactions of 3, 5‐Dimethyl‐4‐Carbethoxy‐2‐Cyclohexen‐1‐One at α‐Position
Authors: Rahman A. U. , Khan M. Y.
Published: June 2015

3, 5‐Dimethyl‐4‐carbethoxy‐2‐cyclohexen‐1‐one has been synthesized through the Knoevenagel condensation1, which is then subjected to alkylation and acylation at α‐position. The resulting products are hydrolyzed and decarboxylated to α‐substituted cyclohexenones. 3, 5‐Dimethyl‐2‐cyclohexen‐1‐one is converted by N‐bromosuccinimide to phenol via enolization2.
The Oxidation and Reduction of 4‐Formyl‐and 4‐Acetyl‐3‐Arylsydnones
Authors: Tien Hsien‐Ju , Yeh Mou‐Yung , Wu Chung‐Hsiung , Chen Hsien‐Tsung
Published: June 2015

A convenient method to prepare methyl 3‐arylsydnonylacetate (I) from 4‐acetyl‐3‐arylsydnone with thallium (III) nitrate by oxidative rearrangement was investigated.

4‐Formyl‐3‐arylsydnones were reduced by sodium borohydride at room temperature to produce 4‐hydroxymethyl‐3‐arylsydnones (II) in moderate yields (65%‐85%), but the corresponding 3‐aryl‐4‐sydnonecarboxaldehyde arylhydrazone (III) was obtained by the electrolytic reduction.
A Convenient Synthesis of N‐Substituted 1,6‐Dihydro‐3(2H)‐Pyridinones
Authors: Chen Ling‐Ching , Wang Eng‐Chi , Lin Jen‐Hom , Wu Shihn‐Sheng
Published: June 2015

N‐Substituted 1,6‐dihydro‐3(2H)‐pyridinones have been synthesised from N‐substituted piperidine‐3,5‐diones via the methyl enol ethers. Reduction of the latter with sodium borohydride (NaBH4) is described.
Synthesis of Methyl‐2, 3‐Di‐O‐Methyl 6‐Deoxy‐3‐C‐Methyl‐a‐D‐Gulopyranoside
Authors: Rahman A. U. , Hong N. , Yoshimura J.
Published: June 2015

Methyl 2,2‐di‐O‐methyl‐6‐C‐methyl‐α‐D‐gulopyranoside has been synthesized from D‐glucose. The introduction of methyl branching at 3‐position was achieved by the Grignard reaction.
Synthesis of Some Dialkyl Bromo‐Substituted Benzyl Phosphonates
Authors: Liaw Ben‐Ruey , Guo Wen‐Jeng
Published: June 2015

Arbuzov reaction of bromo‐substituted benzyl bromides and trialkyl phosphites in benzene gave high yields of dialkyl bromo‐substituted benzyl phosphonates, and —CH2CH2CH2CH3). The structural assignments of these phosphonates were confirmed by 1H nmr, 13C nmr, ir and mass spectral analysis.
Some Reactions of 5‐(3 or 4‐Pyridyl)‐1,3,4‐Oxadiazoles with Amines and Hydrazines
Authors: Zayed S. A. , Fakhr I. E. , Gad F. A. , Abdulla A.
Published: June 2015

2‐Amino‐and 2‐hydrazino‐5‐(3 or 4‐pyridyl)‐1, 3, 4‐oxadiazoles [IIi‐k] have been prepared by racting 2‐chloro derivatives with the corresponding amines or hydrazines, the 2‐hydrazino (IIi‐k) compounds that obtained were heated with carbon disulphide and alcoholic potassium hydroxide where 5‐(3 or 4‐pyridyl)‐1,3,4‐oxadiazolo (2,3‐C)‐1,2,4‐triazole 5‐thione (IIIa‐c) were obtained, the given structures were biologically screened.
A Study of the Nitroso Spin Adducts of the Pentacarbonyl Rhenium Radical
Authors: Chen H. S. , Chen C. P.
Published: June 2015

Nitrosobenzene (NB) and nitroso‐tetr‐butane (NtB) were used to trap the photogenerated rhenium pentacarbonyl radical. Self trapped radicals and spin adducts were studied in detail by EPR spectroscopy. In methylene chloride, both nitroxide and anilino spin adducts can be observed with NtB at −30°. In contrast, only the nitroxide spin adduct of nitrosobenzene was observed in either hexane, or methylene chloride solution. This solvent controlled spin adduct chemistry, can be explained in terms of the solute‐solvent interaction.
Mössbauer Spectroscopic Studies of Supported α‐Fe2O3 and Fe Catalysts II: The Effect of the Second Metal Addition
Authors: Wei Ho‐Hsiang , Lin Kuen‐Hai
Published: June 2015

The effect of the addition of a second metals such as Zn and Ni on the calcinaton and reduction of alumina, magnesia and silicasupported iron catalysis with total iron loading of 5wt% is investigated by Mössbauer spectroscopy. It is shown that the reducibility of supported α‐Fe2O3 is gradually increased by adding the second metal. The values of the magnetic hyperfine field obtained from Mössbauer spectra for the Zn or Ni‐added α‐Fe2O3 or Fe catalysts decreased with increasing second metal loading.
Preparation of Enamines Catalyzed by Lewis Acids in the Presence of Solid Supports
Authors: Chou Shang‐Shing P. , Chu Cheng‐Wu
Published: June 2015

A simple and effective preparation of enamines from bulky ketones and secondary amines has been achieved with the aid of Lewis acid on various solid supports. The optimized yields were higher than those obtained without the solid support. Factors affecting the yield and regioselectivity of these reactions were also studied. Evidence showed that the reaction proceeded simultaneously in solution and on the solid support.
Some Reactions of Chalcone‐4‐Sulfonyl Chloride and 4‐Methoxychalcone‐3‐Sulfonyl Chloride
Authors: Cremlyn Richard J. , Swinbourne Frederick J. , Shode Olufemi O.
Published: June 2015

Chalcone and 4‐methoxychalcone react with chlorosulfonic acid to give chalcone‐p‐sulfonyl chloride and 4‐methoxchalcone‐3‐sulfonyl chloride respectively. The sulfonyl chlorides were converted into 13 sulfonyl derivatives by reaction with nucleophiles. With hydrazine and phenylhydrazine the chalconesulfonyl chlorides were cyclised to the corresponding hydrazinopyrazolines. In contrast, with N,N‐dimethyl‐hydrazine only the dimethylsulfonohydmides were obtained, and no attack on the carbonyl group was observed. Possible reasons for this difference in behaviour are discussed, together with spectroscopic evidence for the structures proposed.
Synthesis of 1‐Acyl‐3‐Piperidones
Authors: Chen Ling‐Ching , Wang Eng‐Chi , Lin Jen‐Hom , Wu Shihn‐Sheng
Published: June 2015

The 1‐acyl‐3‐piperidones (5 and 8) have been synthesised from N‐benzylpiperidine‐3,5‐dione (1) via a reaction sequence, which is shown to be of general utility for the preparation of 1‐acyl‐3‐piperidones. The total yields of 5 and 8 obtained from 1 are 35% and 31% respectively.