Preparation, Characterisation and Thermal Properties of Hydrazinium Magnesium Sulfate

Hydrazinium magnesium sulfate, (N2H5)2Mg(SO4)2, has been prepared by dissolving magnesium powder in a solution of ammonium sulfate in hydrazine hydrate, by the reaction of ammonium magnesium sulfate with hydrazine hydrate, and by the cocrystallisation of dihydrazinium sulfate and magnesium sulfate. The product has been characterized by chemical analysis and infrared spectra. Thermal analysis of (N2H5)2Mg(SO4)2 by TG and DTA show exothermic decomposition at 302°C giving Mg(N2H4)SO4 as an intermediate and an endother-mic decomposition at 504°C producing MgSO4.

Preparation, properties and metabolism of retinoic acid anhydride.

A new analogue of vitamin A, viz., retinoic acid anhydride was prepared, for the first time, by the action of thionyl chloride on retinoic acid in benzene containing pyridine. The amhydride was charcterised by its chromatographic properties, elemental analysis, ultraviolet absorption, infrared and nuclear magnetic resonance spectral characteristics. The compound could be readily hydrolysed to retinoic acid both by acid and alkali treatments and reduced by lithium aluminium hydride to vitamin A alcohol (retinol). The spectral changes with antimony trichloride reagent were similar to those observed for retinoic acid. The metabolism of retinoic acid anhydride was found to be similar to that of retinoic acic. When administered either orally or intraperitoneally, the compound promotes growth in vitamin A-deficient rats. Time-course experiments revealed that retinoic acid anhydride is converted into retinoic acid by non-enzymatic hydrolysis and thereby exerts its biological activity. The biopotency of the anhydride was found to be nearly the same as that of the acid. A new method of preparing esters of retinoic acid employing retinoic acid anhydride as an intermediate, has been described.

Preparation of 1-acyl-2-succinyl glycero-3-phosphorylcholine and evidence against its involvement in succinate dehydrogenase action

1-Acyl-2-succinyl glycero-3-phosphorylcholine (GPC) was synthesized and its properties described. Although 1-acyl-2-succinyl GPC is a good substrate for succinate dehydrogenase, experiments on the incorporation of [2,3-14C]succinate into mitochondrial lipids gave no evidence to indicate that it is an intermediate in the enzymic oxidation of succinate to fumarate, as has been suggested earlier.

Investigations on the preparation, oxidation and reduction reactions of thiophosphoryl fluoride

Pure thiophosphoryl fluoride has been prepared by the fluorination of thiophosphoryl chloride by sodium fluoride in acetonitrile medium. Oxidation of this phosphoryl fluoride by acidified chloramine-T ruptures the phosphorus-sulphur bond and oxidises the sulphur present to the hexavalent state. Anhydrous hydrogen iodide reduces the sulphur to hydrogen sulphide and phosphorus to the trivalent state.

Preparation, IR and nuclear magnetic resonance studies on the rare-earth perchlorate complexes of 3-methylpyridine-1-oxide

THE COMPLEXES of pyridine-l-oxide and 2- and 4-substituted pyridine-l-oxides have been investigated previously[l]. The complexes of 3-substituted pyfidine-l-oxides, however, have received little attention. The rare-earth complexes of pyridine-Ioxide[l, 2], 4-methylpyridine- l-oxide [1] and 2,6- dimethylpyfidine-l-oxide[3,4] have been reported earlier. The present paper deals with the isolation and characterisation of 3-methylpyridine-l-oxide (3-Picoline-N-oxide, 3-PicNO) complexes with rare-earth perchlorates.

Rapid synthetic routes to prepare LiNi1/3Mn1/3Co1/3O2 as a high voltage, high-capacity Li-ion battery cathode material

LiNi1/3Mn1/3Co1/3O2, a high voltage and high-capacity cathode material for Li-ion batteries, has been synthesized by three different rapid synthetic methods. viz. nitrate-melt decomposition, combustion and sol-gel methods. The first two methods are ultra rapid and a time period as small as 15 min is sufficient to prepare nano-crystalline LiNi1/3Mn1/3Co1/3O2. The processing parameters in obtaining the best performing materials are optimized for each process and their electrochemical performance is evaluated in Li-ion cells. The combustion-derived LiNi1/3Mn1/3Co1/3O2 sample exhibits large extent of cation mixing (10%) while the other two methods yield LiNi1/3Mn1/3Co1/3O2 with cation mixing <5%. LiNi1/3Mn1/3Co1/3O2 prepared by nitrate-melt decomposition method exhibits superior performance as Li-ion battery cathode material.

A New Method for the Preparation of Sulphuryl Chloro Fluoride

It has been observed that a suspension of sodium fluoride in boiling acetonitrile could be used for the preparation of fluorine compounds such as silicon tetrafluoride [1], thiophosphoryl fluoride [2], sulphur tetrafluoride [3,4], and fluorocyclophosphazenes [5]. This method, when adopted for the fluorination of sulphuryl chloride [6], it is observed that a mixture of sulphuryl fluoride and sulphuryl chloro fluoride is obtained. On the other hand, when lead fluoride is substituted for sodium fluoride, pure sulphuryl chloro fluoride is evolved. Based on this observation, a new method has been standardised for the preparation of a pure sample of sulphuryl chlorofluoride by fluorinating sulphuryl chloride by lead fluoride in acetonitrile medium.

Pyridinium poly(hydrogen fluoride)- a reagent for the preparation of hexafluorophosphates

Pyridinium poly(hydrogen fluoride) has been found to be an efficient and versatile reagent for the preparation of hexafluorophosphates. Pyridinium hexafluorophosphate has been prepared by the reaction between phosphorus (V) halides (POCl3, POBr3, PSCl3, PCl5, PBr5) and pyridinium poly(hydrogen fluoride). This in turn is used to prepare the hexafluorophosphates of ammonium, sodium, potassium, rubidium and cesium in good yield and high purity.

A simple method for large-scale preparation of chick embryo tRNA

A simple method for preparing bulk quantities of tRNA from chick embryo has been developed. In this method chick embryos were homogenized in a buffer of pH 4.5, followed by deproteinization with phenol. The aqueous layer was allowed to separate under gravity. The resulting aqueous layer, after two more phenol treatments, was directly passed through a DEAE-cellulose column and the tRNA eluted therefrom with 1 Image NaCl. The tRNA prepared by this method was as active as the one prepared at neutral pH.

Preparation of Palladium(II) Complexes of Isonitrosoacetylacetoneimines Having O- and N-Coordinated Isonitroso Groups

Methods for the preparation of palladium(II) complexes of the type Pd(R-IAI)(IAI'), where IAI' is the anion of isonitrosoacetylacetoneimine and R-IAI, its N-alkyl or N-aryl derivative, are given.

Effect of the method of preparation and pretreatment on the texture of alumina and related catalysts

The effect of the method of preparation and pretreatment on catalyst texture was investigated in the case of alumina, silica-alumina, 10 × molecular sieve and thoria catalysts. All the catalysts were characterised with respect to their specific surface area, surface acidity, pore size distribution and pore volume. The above properties were found to reflect the textural changes that might have been undergone by the catalyst surface as a result of the method of preparation and pretreatment. The method of preparation was found to influence markedly the acidity of the surface and to a lesser extent the surface area and pore size distribution. Acid-treatment was found to increase selectively the acidity of the catalyst while heat-treatment was found to decrease proportionally the acidity as well as surface area of the catalyst.

Preparation and x-ray characterization of four new crystal forms of Jacalin, a lectin from Artocarpus integrifolia

Four new crystal forms of the anti-T lectin from jackfruit (Artocarpus integrifolia) have been prepared and characterized. Three of them, two monoclinic (P21, A = 59·4 Å, B = 83·3 Å, C = 63·5 Å, β = 107·7°; C2, A = 106·1,Å, B = 53·9 Å, C = 128·0 Å, β = 95·0 Å) and one orthorhombic (C2221, A = 98·1 Å, B = 67·3 Å, C = 95·1 Å) were grown with 2-methylpentan-2,4-diol (MPD) as the precipitant while the fourth, an hexagonal from (P6122, A = b = 129·6 Å, C = 157·9 Å), was obtained in the presence of methyl-ga-Image -galactopyranoside with polyethylene glycol 4000 as the precipitant. The reported relative molecular mass (Mr) of the lectin was found to be inconsistent with the solvent content of the crystals estimated using measured densities. The Mr was redetermined using size-exclusion chromatography in the presence of methyl-α-Image -galactopyranoside and Ferguson-plot analysis of mobilities in polyacrylamide gel electrophoresis. The redetermined Mr (66,000) is consistent with the measured crystal densities. The orthorhombic and the hexagonal forms, which have one half molecule and one molecule, respectively, in the asymmetric unit, are suitable for high-resolution X-ray analysis.

Rapid quenching and glass formation in chalcogenide glasses: Preparation and properties of Ge-As-Te glasses over an extended composition ranges

In Ge-As-Te system, the glass forming region determined by normal melt quenching method has two regions (GFR I and GFR II) separated by few compositions gap. With a simple laboratory built twin roller apparatus, we have succeeded in preparing Ge7.5AsxTe92.5-x glasses over extended composition ranges. A distinct change in T-g is observed at x = 40, exactly at which the separation of the glass forming regions occur indicating the changes in the connectivity and the rigidity of the structural network. The maximum observed in glass transition (T-g) at x = 55 corresponding to the average coordination number (Z(av)) = 2.70 is an evidence for the shift of the rigidity percolation threshold (RPT) from Z(av) = 2.40 as predicted by the recent theories. The glass forming tendency (K-gl) and Delta T (=T-c-T-g) is low for the glasses in the GFR I and high for the glasses in the GFR II.

A Remarkably Simple One-Step Procedure for the Preparation of alpha-Bromo-alpha,beta-Unsaturated Carbonyl Compounds

An easy and convenient one-step procedure for the conversion of alpha,beta-unsaturated carbonyl compounds into their corresponding bromo-enones using NBS-Et3N center dot 3HBr in the presence of potassium carbonate in dichloromethane at 0 degrees C to room temperature under very mild conditions in high yields and significantly shorter times, is reported.