Search results for "Azide"

Synthesis and Derivatization of Substituted (R)- and (S)-C-Allylglycines

2004

Various (R)- and (S)-C-allylglycine derivatives were synthesized by means of an auxiliary controlled diastereoselective aza-Claisen rearrangement. Starting from (S)-configured auxiliaries derived from optically active proline, an aza-Claisen rearrangement enabled us to synthesize α(R)-configured γ,δ-unsaturated amides. Since (R)-allylglycine derivatives could be directly generated by reacting N-allylproline derivatives and various protected glycine fluorides, the corresponding (S)-enantiomers were built-up via an initial α-chloroacetyl chloride rearrangement and a subsequent chloride azide substitution with complete inversion of the configuration. High diastereoselectivities were obtained (…

Performance of micellar mobile phases in reversed-phase chromatography for the analysis of pharmaceuticals containing beta-blockers and other antihyp…

1996

A rapid and simple reversed-phase micellar liquid chromatographic procedure for the simultaneous determination of the beta-blockers atenolol, metoprolol and oxprenolol, the diuretics amiloride, bendroflumethiazide, chlorthalidone and hydrochlorothiazide and the vasodilator hydralazine in pharmaceuticals, is proposed. An interpretive optimization procedure, which uses the chromatographic data for only five mobile phases, was applied to select a suitable micellar mobile phase. A comparative study was also made of the performance of micellar and aqueous-organic mobile phases in the analysis of pharmaceuticals that combine beta-blockers and diuretics. The determination of all the drugs could be…

Solid-Phase Extraction Techniques for Assay of Diuretics in Human Urine Samples

1991

Abstract Solid-phase extraction techniques were evaluated for the treatment of urine samples in the analysis of diuretics before injection into an HP-Hypersyl ODS-C18 column. Six different reversed-phase extraction columns were tested, and the results obtained are compared with those obtained in a classical liquid-liquid extraction with ethyl acetate. The solid-phase extraction procedures are the best overall choice for all the diuretics tested, due to their versatility, the minor time-consuming, and the good recovery percentages obtained. C18 and C8 packings give the highest recoveries for a majority of the diuretics studied. However, CH or PH columns, due to their greater selectivity, can…

Evaluation of several global resolution functions for liquid chromatography

1999

Abstract An interpretative approach, that makes use of the overlapped fraction of each chromatographic peak as elementary resolution criterion, was applied to the separation of mixtures of compounds. The elementary resolution measurements for all peaks in the chromatogram were reduced to a single numerical value using several functions: normalised by the mean resolution product, unnormalised product, geometrical mean of the unnormalised product, and worst elementary resolution value. The descriptive capability of these reduction functions was evaluated through the observation of global resolution diagrams and the change in the shape of the chromatograms in the selected factor space. michrom…

Spectrophotometric Determination of Hydralazine with 2-Hydroxy-1-naphthaldehyde in Pharmaceuticals

1991

Abstract A new extraction-spectrophotometric method for the determination of hydralazine, based on its reaction with 2-hydroxy-1-naphthaldehyde at 25 °C, is described. The calibration curve was linear between 0.4 and 6 mg/mL of hydralazine. The molar absorbtivity of the product at 408 nm is 40 900 L · mol − 1 · cm − 1 . The method described was applied to the analysis of hydralazine in pharmaceutical preparations containing reserpine, hydrochlorothiazide, bendrofluorthiazine, propranolol, and other substances. The agreement with the U.S.P. XXI method was satisfactory for tablets and injections, but not for pellets.

Molecular, Supramolecular Structures Combined with Hirshfeld and DFT Studies of Centrosymmetric M(II)-azido {M=Ni(II), Fe(II) or Zn(II)} Complexes of…

2021

The supramolecular structures of the three metal (II) azido complexes [Fe(4bzpy)4(N3)2]

A new tetranuclear defective dicubane azide-bridged cobalt(II) complex

2013

Abstract The new tetranuclear cobalt(II) complex with formula [Co4(N3)8(4,5-diazafluoren-9-one)4] (1) is reported. Complex 1 is a cobalt(II) defective dicubane azide-bridged compound showing only azido bridging ligands in the μ1,1– and μ1,1,1– coordination modes. The magnetic properties of 1 are reported. Magnetic susceptibility measurements indicate ferromagnetic coupling. The magnetic data have been fitted to 2 K by considering two different superexchange coupling constants. The out-of-phase signal χM″ displays frequency-dependence below approximately 9 K.

Characterisation and reactions of molecular cesium azide

2006

Preparation, crystal structure and magnetic properties of di-2-pyridylamine (dpa) copper(II) complexes [Cu(dpa)(N3)2]n and [Cu2(dpa)2(NCO)4]

2008

Abstract The preparation, crystal structures and magnetic properties of two copper(II) complexes with di-2-pyridylamine (dpa) as end-cap ligand and azide (1) and cyanate (2) as bridging groups, [Cu(dpa)(N3)2]n (1) and [Cu2(dpa)2(NCO)4] (2), are reported. Compound 1 consists of uniform chains of copper(II) ions bridged by single μ-1,1-azido groups whereas that of compound 2 is made up of centrosymmetric dicopper(II) units with double μ-1,1-N-cyanate bridges, the other two cyanate groups acting as terminal ligands. The copper atoms in 1 and 2 are five-coordinated with two nitrogen atoms of a bidentate dpa ligand (1 and 2), one nitrogen atom from a terminally bound azide (1)/cyanate (2) and tw…

Mechanismus der Umsetzung von 1,1-Diphenylhydrazin mit Azodicarbonsäure-diethylester

1979

Bei der Umsetzung von 1,1-Diphenylhydrazin (1a) mit Azodicarbonsaure-diethylester (2a) uber-lagern sich funf Reaktionsmechanismen: A und B) Oxidation des Diphenylhydrazins 1a durch den Azodicarbonsaureester 2a zum Aminonitren 8; Bildung des Tetrazens 10 entweder durch Dimerisierung von 8 oder uber das Tetrazan 11; Zerfall von 11 in N2 und Diphenylamin. — C) Addition des Aminonitrens 8 an den Azodicarbonsaureester 2a zum Aminoazimin 3a; Zerfall von 3a in das Urethan 4a und den Azidoameisensaureester 5a. — D) Isomerisierung des Aminoazimins 3a zu 13 und Reduktion von 13 durch 1a zum Tetrazen 14; Spaltung von 14 in Diphenylamin und das Azid 15; Zerfall von 15 in Ethylcyanat (17) und den Kohlen…