Application of sodium metaperiodate for the determination of ribavirin in pharmaceutical formulations

Three simple and sensitive visible spectrophotometric methods (A-C) have been described for the assay of ribavirin either in pure form or in pharmaceutical formulations. They are based on the oxidation of ribavirin with excess sodium metaperiodate and estimating either the products formed (dialdehyde with MBTH, method A; iodate with metol-sulphanilamide, in the presence of Mo(VI) and iodide, method B) or the amount of periodate consumed (celestine blue in the presence of telurium (IV), method C). All of the variables have been optimized and the reaction mechanisms presented. The concentration measurements are reproducible within a R.S.D. of 1.0%. Recoveries are 99.2-101.2%.     

K α L 1 satellite multiplet structure of photon-excited chlorine atoms

Summary An attempt is made to study theK _α L ¹ satellite multiplet structure of chlorine atoms in different compounds by photon excitation. A comparison of the averageK _α L ¹ group energy shift from the diagram line with those based on Dirac-Fock evaluations with different number ofM-shell electrons shows a reasonable agreement. The intensity ratios are found to be higher than those studied in Mg compounds in general.     

Thallimetric oxidations-V Titrimetric and spectrophotometric determination of hydrogen peroxide

Titrimetric and spectrophotometric methods have been developed for the determination of hydrogen peroxide at mmole and mumole levels respectively. In these methods thallium(III) is used as the oxidant and the reduced thallium(I) is determined oxidimetrically with potassium bromate in the titrimetric method and by measuring the absorbance of thallium(III) at 260 nm in the presence of 0.1M hydrochloric acid and 1M perchloric acid in the spectrophotometric method. Photochemical redox methods for the estimation of hydrogen peroxide in the presence of a number of diverse ions are described.     

Reductive etherification of carbonyl compounds with alkyl trimethylsilylethers using polymethylhydrosiloxane (PMHS) and catalytic B(C6F5)3

A facile synthesis of symmetrical and unsymmetrical ethers is achieved by reductive coupling of carbonyl compounds with alkoxysilanes. This reaction is performed using inert polymethylhydrosiloxane as the hydride source and B(C₆F₅)₃ as the catalytic activator of the PMHS.     

Synthesis of homoallylic chiral tertiary alcohols via chelation-controlled diastereoselective nucleophilic addition on alpha-alkoxyketones: application for the synthesis of the C(1)-C(11) subunit of 8-epi-fostriecin

[reaction: see text] Chiral beta-syn-alkoxyhomoallylic alcohols derived from alkoxyallylboration of aldehydes upon oxidation provided the corresponding chiral ketones. Chelation-controlled nucleophilic addition to these ketones occurred in a highly stereoselective manner to afford anti-homoallylic tertiary alcohols. This methodology has been applied for the synthesis of the C(1)-C(11) subunit of C(8)-epi-fostriecin.     

Reactivity ratios of ethyl acrylate,n-butyl methacrylate copolymer system by 1H-NMR

Ethyl acrylate (EA) and n-butyl methacrylate (n-BMA) copolymers were prepared in solution and the composition of the copolymer samples was estimated by ¹H-NMR spectroscopic techniques. Because the characteristic signals, which vary with the composition of the copolymer, were absent, the ratio of intensities of down-field protons to that of the total protons was used for the estimation of copolymer composition. Reactivity ratios were calculated from these values by using the Kelen-Tudos differential linear equation.     

Oxine complex of molybdenum

Molybdenum was reported to be precipitated quantitatively by 8-hydroxyquinoline in the pH range 3.3–7.6, the precipitated compound having the composition MoO₂(ox)₂. The pH range reported and the composition of the complex do not seem to be compatible with present knowledge of the pH stability of anionic and cationic molybdenum. It is now shown that under defined conditions, the precipitate is not formed at pH values higher than 2.24. In several estimations of other metals, molybdenum was masked by using a complexone at high pH values. It is now pointed out, that maintaining the solution at high pH value is itself sufficient and no other external complexing agent is necessary for masking molybdenum.     

A novel conversion of erythro phospholane epoxides to one-carbon atom homologated allylic alcohols

A novel synthetic approach is described to incorporate one more carbon atom at C-2 position of phospholane oxides as homologated allylic alcohol by treatment of erythro-2,3-epoxy-3-methylphospholane 1-oxides with excess of dimethylsulfonium methylide.     

Cu(I)-mediated deoxygenation of N-oxides to amines

A mild and highly efficient deoxygenation of variety of N-oxides using an inexpensive CuX, or a CuX-Zn or CuX-Al couple is described.