Racemates of (η3-allyl)tricarbonyliron lactone complex Fe(CO)3{η1:η3-C(O)XCH2CHCMeCH2} 1a (X = O) and (η3-allyl)tricarbonyliron lactam complex 2a (X = NMe) are resolved on a preparative scale by HPLC on cellulose tris(3,5-dimethylphenyl)carbamate/silica gel RP-8 and the absolute configuration of (-)-2a is determined by X-ray crystal structure analysis.
Abstract
Sulfaquinoxaline is determined by its UV absorbance at about 358 nm, where the other 3 sulfonamides do not absorb. Sulfathiazole, sulfamerazine, and sulfamethazine are determined by a quantitative TLC procedure, based on the separation of the compounds on silica gel plates; the spots are extracted and the centrifuged extracts are analyzed spectro-photometrically. A method of calculating the total sulfonamide content, independent of the individual components, is also introduced.
Preparative-scale HPLC Resolution of Metallacyclic η3-Allyltricarbonyliron Complexes and Determination of the Absolute Configuration by X-Ray Crystal Structure Analysis