Synthesis,spectral characterization and catalytic applications of Ru(II) complexes with amide ligands

Ruthenium(II) complexes of the type, RuCl₂(NO)(PPh₃)(L₂) (where L = amide ligand) have been synthesized and characterized on the basis of their elemental analysis IR, ¹H-, ¹³C-, ³¹P-NMR spectra. Amide ligand behaved as a bidentate ligand. The probable structures of these complexes have been discussed. They were used as catalysts for the hydrolysis of drugs viz. rivastigmine tartrate and neostigmine bromide. The percent yields of hydrolyzed products of these drugs were determined spectrophotometrically.     

Study on using high injection voltage and spiral inflector in the central region of VEC

A feasibility study of using high injection voltage and spiral inflector in the present heavy ion central region of VEC is described. Conditions necessary for waist-to-waist transfer of the ion beam in the hole lens of main magnet have been obtained. The results of orbit studies of a variety of heavy ions indicate that a spiral inflector can be used in the central region.     

Copper nitrate trihydrate catalyzed efficient synthesis of bis(indolyl)methanes in acetonitrile at room temperature

A catalytic amount of easily available and inexpensive Cu(NO₃)₃.3H₂O (10 mol%) enables electrophilic substitution reaction of indole with structurally divergent aldehydes in acetonitrile to afford the corresponding bis(indolyl)methanes in moderate to excellent yields (65‐98%) at ambient temperature. The reaction is highly chemoselective and applicable only to aldehydes and not to ketones.     

Synthesis, spectral studies and antibacterial activity of novel macrocyclic Co(II) compounds

Ten novel macrocyclic Co(II) compounds have been synthesized by treating four N(4) and six N(2)O(2) donor macrocycles with cobalt chloride in methanol. These compounds were characterized by elemental, IR, (1)H, (13)C NMR, mass, electronic spectral analysis, molar conductance and magnetic susceptibility measurements. Thermal behavior of these compounds has been studied by the thermogravimetric analysis. An octahedral geometry has been proposed for all of these complexes. All the macrocycles and macrocyclic Co(II) compounds along with existing antibacterial drugs were screened for antibacterial activity against Gram +ve and Gram -ve bacteria. All these compounds were found to be more active when compared to streptomycin and ampicillin.     

Ruthenium(III) chloride-catalyzed efficient protocol for ethyl diazoacetate insertion into the N–H bond of secondary amines

Ruthenium(III) chloride (1 mol%) alone can catalyze the insertion of ethyl diazoacetate into N–H bonds of various structurally and electronically diverse secondary cyclic amines under solvent-free conditions to afford the corresponding glycine esters in good yields under ambient conditions. Reactions with various aliphatic primary and aromatic amines examined, however, were unsuccessful. Correspondence: Dr. Srinivas R. Adapa, Indian Institute of Chemical Technology, Hyderabad 500 007, India.     

Validated Chromatographic Methods for the Determination of Process Related Toxic Impurities in Pantoprazole Sodium

A GC–MS method for the simultaneous determination of two process related toxic impurities viz. 2-(chloromethyl)-3,4-dimethoxypyridine hydrochloride (CDP) and dimethyl sulfate (DMS) and RP-LC for the routine determination of CDP in pantoprazole sodium (PPS) are presented. In GC–MS, a temperature gradient program was performed on a capillary DB-624 column (60 m × 0.32 mm × 1.8 μm). LC analysis of CDP was done on a Novaflex C18 (250 × 4.6 mm, 5 μm) column using mobile phase containing buffer (0.02 M potassium dihydrogen phosphate and 0.0025 M di potassium hydrogen phosphate) and acetonitrile in 46:54 v/v ratio. The flow rate was 1.0 mL min^?1 and the elution was monitored at 220 nm. Both methods were validated as per International Conference on Harmonization (ICH) guidelines. GC–MS is able to quantitate up to 3.0 ppm of CDP and DMS whereas with RP-LC up to 9.0 ppm of CDP could be quantitated.     

Molecular iodine-catalyzed efficient N-Cbz protection of amines

An efficient and selective protection of various structurally and electronically divergent aryl and aliphatic amines with Cbz-Cl in the presence of a catalytic amount of molecular iodine (2 mol%) in methanol with high yields at ambient temperature is presented.     

Analytical Studies on the Role of Oxidants of the Olefinic Double Bond in the Determination of Flunarizine

Simple, sensitive, and selective spectrophotometric methods (M₁ and M₂) for the assay of flunarizine (FZ) through the olefinic double bond are proposed. Method M₁ is based on the reaction of potassium permanganate to the olefinic double bond in FZ and estimating the unreacted permanganate with Fast Green FCF (FG FCF). Method M₂ involves the treatment of the olefinic double bond in FZ with a Lemieux reagent (KMnO₄ and NaIO₄) and estimating the aldehyde formed with 3-methyl-2-benzothiazolinone hydrazone (MBTH). The color produced in both methods has maximum absorption at 620 nm. The Beer's law limits, precision, and accuracy of the methods are checked by the reference method. The methods are found to be suitable for the determination of flunarizine. The recoveries range from 99.18 to 101.13%.