New methods for the preparation of 1-phenyl-trans-cyclohexane-1,2-diol

In contrast with previous reports, it was found that the reaction of 1-phenylcyclohexene with peroxyformic acid is not entirely stereospecific, but gives some trans-1-phenylcyclohexane-1, 2-diol (IV) beside the cis-isomer (III). The reaction of 1-phenylcyclohexene oxide (II) with formic acid yielded a similar mixture of III and IV, while addition of trichloroacetic acid in benzene was entirely cis-stereospecific. Reaction of the epoxide II with potassium hydroxide took place only under very drastic conditions to give a small yield of III, while sodium 2-dimethylaminoethoxide added exclusively in a trans way, leading to the amino ether X, which was easily transformed into the trans-glycol IV. The latter compound was also the main product of the borohydride reduction of 2-hydroxy-2-phenylcyclohexanone (IX). Possible explanations of the observed stereochemical results are discussed.     

Inorganic complexes in volumetric analysis. Part III. Use of ferric fluoride complex in the estimation of iodide

Summary The method for estimation of iodide formulated in the earlier publications of the series bas been modified by the use of sodium fluoride as the complexing agent in the place of oxalate or phosphoric acid. The results obtained are in excellent agreement with the calculated ones and the method has been successfully applied for the estimation of iodide in iodized salt.     

Asymmetric hydrogenation in the presence of bicyclic chiral phosphines

Both enantiomers of trans-2,3-diphenylphosphinomethyl-norbornene-(5), prepared by two independent synthetic routes, were used as ligands in the asymmetric hydrogenation of -acetamidocinnamic acid in the presence of rhodium(I). Small variations in the ligand structure have a remarkable influence on the activity of the catalytic system.

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-2,3----(5), , - (I). .

     

Isolation of ribosomes from cotton seeds

Summary 1. It has been established that the method of precipitation with ethanol in the presence of an increased concentration of Mg²⁺ can be used for the rapid isolation of the ribosome fraction from plant material.2. The optimum conditions for the complete precipitation of the ribosome fraction from a homogenate of cotton seeds have been selected.3. By treating an extract of the seeds with 0.5 M KCl it was possible to reduce the amount of tRNA in a preparation of the total rRNA.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 852–856, November–December, 1977.     

Spot tests for calcium sulphate, lead sulphate, silver, thallium, and formaldehyde based on reactions with selenosulphate

Summary Spot tests have been described for calcium sulphate, lead sulphate, silver, thallium and formaldehyde based on the reaction with selenosulphate. In these reactions either red elemental selenium (CaSO₄, CH₂O) or black metal selenide (PbSO₄ Tl, Ag) is formed. The limits of identification are: 0.2 mg of PbS04 or CaSO₄, 2 g of Ag, 10 g of Tl, 0.2 g of CH₂O.

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Zusammenfassung Für Calciumsulfat, Bleisulfat, Silber, Thallium und Formaldehyd werden Tüpfelproben beschrieben, die auf Umsetzungen mit Selenosulfat beruhen. Hierbei -wird entweder rotes elementares Selen abgeschieden (CaSO₄ CH₂O) oder schwarze Selenide werden gebildet (PbSO₄, Tl, Ag). Die Nachweisgrenzen betragen: 0,2 mg PbSO₄ oder CaSO₄, 2 g Ag, 10 g Tl, 0,2 g CH₂O.

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This paper has been dedicated to Prof. Dr.Fritz Wessely, Vienna, on the occasion of his 70th birthday.     

Gravimetric determination of thorium and zirconium

Summary Thorium and zirconium can be quantitatively precipitated by quinaldinic acid atph 2.7 and 3, respectively. As the precipitates are of nonstoichiometric composition they are to be ignited to oxides. By this reagent thorium can be quantitatively separated from arsenic (As³⁺), mercury (Hg²⁺), rare earths, manganese, magnesium and alkaline earths and zirconium from all the aforesaid ions excepting rare earths which contaminate to a slight extent.     

The potentiometric and amperometric determination of silver with mercaptophenylthiothiadiazolone and mercaptobenzthiazole

Summary The previously described gravimetric determinations of silver were used for the potentiometric and amperometric determinations of silver in the presence of interfering cations. The potentiometric titration of silver with MFTD (MBT) is a simple matter, if enough complexone is present, in both ammoniacal and neutral solutions. The amperometric determination of silver with MFTD (MBT) is carried out in neutral solution, containing complexone, with rotated platinum electrode and mercury-mercuric iodide half-cell, short-circuited through a microammeter. The only interfering elements are mercury, gold, and some of the platinum metals.     

A physico-chemical study of iron-chromium-molybdenum catalysts

In the study of the Fe_1–xCr_xMo_1·5O₆ system by X-ray, IR and Mössbauer methods the formation of solid state substitution solutions has been detected, which possess similar catalytic properties in methanol oxidation.

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, , Fe_1–xMo_1·5O₆ , .

     

The theory and practice of polarography in melts

Some of the problems of using solid micro-electrodes in molten salts are discussed. The technique of high-temperature polarography is described and some of the anomalous features of the results are examined.