[1,3‐Bis(di­phenyl­phosphino)prop­ane]­tri­chloro­oxorhenium(V)

Tri­chloro­oxo­[1,3‐prop­ane­diyl­bis­(di­phenyl­phosphine)‐P,P′]rhen­ium(V), [Re­Cl₃­O­(C₂₇­H₂₆P₂)], crystallizes with four formula units per unit cell. The crystal structure consists of neutral complexes of [ReOCl₃(dppp)] [dppp is 1,3‐bis(diphenylphosphino)propane] packed by H?π‐ring interactions. The Re atom is octahedrally coordinated to the oxo anion, three Cl atoms and two P atoms from the dppp ligand. The six‐membered ring formed by the bidentate dppp ligand and the rhenium metal centre is in a chair conformation. The title compound is an intermediate in the synthesis of bis(dppp) complexes of rhenium.     

Spectrofluorimetric Assay of Temafloxacin in Pharmaceutical Formulations and in Serum

A simple and rapid assay is described for the determination of temafloxacin, 1-(2,4-difluorophenyl)-6-fluoro-7-(3-methylpiperazin-1-yl) 1,4- dihydro-4-oxoquinolin-3-carboxylic acid hydrochloride, in pharmaceutical formulations and in serum, based on the fluorescence emission of the drug. The assay of pharmaceuticals involves the measurement of fluorescence at 460 nm of the sample diluted in 0.1 H₂SO₄ with an excitation wavelenght of 276 nm and the assay of serum involves the use of the synchronous spectrofluorimetric method. An appropriate selection of the difference between the wavelengts of both monochromators (ΔΛ) allowed the direct and rapid determination of temafloxacin in serum samples without previous extraction. The procedure, which has been shown to be accurate, precise and sensitive requires only 0.25–0.4 ml of serum depending on the drug concentration.     

Spirolactams as conformationally restricted pseudopeptides: synthesis and conformational analysis

The synthesis of 1-(tert-butoxycarbonyl)-7-[1-(tert-butoxycarbonyl)-3-methylbutyl]-6-oxo-1,7-diazaspiro[4.5]decanes (S,S)-1a and (S,R)-1b is described. Derivatives 17a,b and 19a are prepared for use in peptide synthesis as constrained surrogates of the Pro-Leu and Gly-Leu dipeptides. The Ac-[Gly-Leu]-Met-NH(2) derivatives (S,S,S)-2a and (S,R,S)-2b, with the tripeptidic C-terminal region present in tachykinins, are also synthesized. Conformational analyses of these tripetide analogues by NMR experiments and molecular modeling calculations show that both (S,S,S)-2a and (S,R,S)-2b epimers are gamma-turn/distorted type II beta-turn mimetics.