Molar extinction coefficients of solutions of some organic compounds

Molar extinction coefficients of aqueous solutions of some organic compounds, viz. formamide (CH₃NO),N-methylformamide (C₂H₅NO),NN-dimethylformamide (C₃H₇NO),NN-dimethylacetamide (C₄H₉NO), 1,4-dioxane (C₄H₈O₂₄), succinimide (C₄H₅NO₂) and solutions of acetamide (C₂H₅NO) and benzoic acid (C₇H₆O₂) in 1,4-dioxane (C₄H₈O₂) have been determined by narrow beam γ-ray transmission method at 81, 356, 511, 662, 1173 and 1332 keV. The experimental values of mass attenuation coefficients of these compounds have been used to calculate effective atomic numbers and electron densities. The additivity rule earlier used for aqueous solution has been extended to non-aqueous (1,4-dioxane) solutions.     

Direct conversion of tert-butyl 2-hydroxyalkyl sulfides to 1,3-oxathiolanes

tert-Butyl 2-hydroxyalkyl sulfides, prepared by reaction of epoxides with 2-methylpropane-2-thiol, are converted directly to 1,3-oxathiolanes upon treatment with pivalaldehyde and boron trifluoride diethyl etherate in the presence of thioanisole.     

X-ray diffraction (powder), e.s.r. and other spectral studies oftris[methylenebis(diphenylphosphine oxide)]iron(III) perchlorate

Summary Bifunctional methylenebis(diphenylphosphine oxide) (mdpo) on reaction with iron(III) perchlorate forms the complex, [Fe(mdpo)₃](ClO₄)₃ · H₂O. This has been characterized through elemental analysis, i.r., far-i.r., u.v. and visible spectroscopy and by x-ray diffraction, magnetic moment, molar conductance and e.s.r. data. The e.s.r. spectrum consists of five lines with transitions from: ¦–5/2¦–3/2¦–3/2¦–1/2, ¦–1/2¦+1/2¦+1/2¦+3/2 and ¦+3/2¦+5/2 centred at a g-value of 2.00. On the basis of these studies, a chelated octahedral structure has been assigned to the cation, [Fe(mdpo)₃]³⁺.     

Dibromosilylene: Determination of the absolute rate constants for its gas-phase reactions with oxygen and nitric oxide

Following the newly-discovered UV absorption spectrum of Br₂Si, its reactions with oxygen and nitric oxide in the gas phase have been quantitatively investigated using the flash photolysis-kinetic absorption spectroscopy technique. The room temperature bimolecular rate constants are:      

Complexes of metal ions with phosphorus or arsenic containing ligands. Part XVIII. Chelates ofo-phenylenebis(diarylarsines) with cobalt(II) and nickel(II) halides and pseudohalides

Summary Ten complexes of nickel(II) and cobalt(II) witho-phenylenebis(diphenylarsine), (pdpa) ando-phenylenebis(di-p-tolylarsine), (pdta) have been synthesised. The stoichiometry of complexes is markedly dependent upon the reaction temperature, thus reaction atca. 0° gives the M(A-A)₂X₂ chelates, [M = Ni, X = Br, (A-A) = pdpa; M = Ni, X = I, (A-A) = pdpa, pdta; M = Co, X = CNS, (A-A) = pdpa] whereas at higher temperatures the M(A-A)X₂ chelates [M = Ni, X = Br, I, (A-A) = pdpa, pdta; M = Co, X = CNS, (A-A) = pdpa or pdta] are obtained. The Ni(A-A)₂I₂ compounds can be converted into Ni(A-A)I₂ by boiling under reflux in n-BuOH; the conversion can be reversed by cooling a CH₂Cl₂ solution of the latter at or below 0°. Stereochemical assignments of all the new complexes have been made on the basis of room temperature _eff values, molar conductance, i.r. and u.v. data.     

Mössbauer study of the thermal decompositions of alkaline earth tris(oxalato)ferrates(III)

The thermal decompositions of alkaline earth tris(oxalato)ferrates(III) (Mg, Ca, Sr and Ba) have been studied by Mössbauer spectroscopy and other techniques. During the thermal decomposition, dehydration occurs first, followed by reduction to iron(II) species, and oxides and ferrites (MFe^IIIO₄) are then formed at higher temperature. In the case of strontium tris(oxalato)ferrate(III), strontium ferrite (SrFe^IVO₄) is formed at 700°.

---

Zusammenfassung Die thermische Zersetzung von Tris(oxalato)ferraten(III) der Erdalkalimetalle (Mg, Ca, Sr, Ba) wurde durch Mössbauer-Spektroskopie und andere Techniken untersucht. Im Verlaufe der thermischen Zersetzung verläuft zunächst die Dehydratisierung, gefolgt von der Reduktion zu Eisen(II)-Species. Oxide und Ferrite (MFe^IIIO₄) werden danach bei höheren Temperaturen gebildet. Strontium-tris(oxalato)-ferrat(III) geht bei 700 °C in Strontiumferrit (SrFe^IVO₄) über.

---

() () , , ë . , , MFe^IIIO₄. 700° SrFe^IVO₄.

     

Microwave Induced Bismuth Trichloride Catalysed Beckmann Rearrangement of Oximes

A new and efficient method for the rearrangement of oximes 1 has been achieved by a simple reaction of a ketoximes with bismuth trichloride under microwave irradiation in the solid state.     

Microwave Assisted Rupture of Furoxans to Nitrile Oxides and Intermolecular Capture by Dipolarophiles

3,4-Diaroylfuroxans 1 react with various dipolarophiles 3 under microwave activation to afford the cycloadduct 4 instead of the expected isoxazole 5 in good yields in the absence of solvent.     

Ammonium Sulphate—Magnesium Promoted Selective Reduction of Aromatic Nitro Compounds

Various nitroarenes and 2,1,3-benznooxadiazole-1-oxides were selectively and rapidly reduces to their corresponding amino and diamino compounds respectively in high yields using (NH₄SO₄-Mg/A1/Bi, a new reduction system.     

Analytical QbD-based systematic bioanalytical HPLC method development for estimation of quercetin dihydrate

The current work entails development of rapid, sensitive, and inexpensive high-performance liquid chromatographic method of quercetin dihydrate using the quality by design approach. Quality target method profile was defined and critical analytical attributes (CAAs) were earmarked. Chromatographic separation was accomplished on a C₁₈ column using acetonitrile and ammonium acetate buffer (35:65) %v/v (containing 0.1% acetic acid, pH 3.5) as mobile phase at 0.7?mL/min flow rate with UV detector at 237?nm. Screening studies using fractional factorial design revealed that organic modifier, injection volume, column temperature, and buffer strength have significant influence on method CAAs, namely, peak area, retention time, and peak tailing. The critical method parameters were systematically optimized using Box–Behnken design. Response surface mapping was used along with numerical optimization and desirability function for identifying the optimal chromatographic conditions. Linearity was observed in the drug concentration ranging between 2 and 50?µg/mL. Accuracy analysis revealed mean % recovery between 93.6 and 96.2%, while precision study revealed mean % recovery between 93.7 and 96.5%. Limits of detection and quantification of the developed method were found to be 12.1 and 36.6?ng/mL. Overall, the studies construed successful development of chromatographic method of quercetin with enhanced method performance.