Determination of acetone, 2-butanone, diethyl ketone and BTX using HSCC-UV-IMS

A combination of a custom-designed ion mobility spectrometer (IMS) with a UV ionization source and a high speed capillary column (HSCC) has been developed as an analytical device for the sensitive detection of volatile organic compounds (VOCs), e.g. 2-propanone (acetone), 2-butanone and 3-pentanone (diethyl ketone) in the gas phase. A fast separation of the three selected substances and benzene, toluene and m-xylene (BTX) - all of which occur in human breath - has been achieved within less than four minutes at a carrier gas flow rate of 4.5 mL x min(-1). Multi-dimensional correlations presented support the interpretation of the acquired spectra of mixtures. Method detection limits were 2.7 microg x L(-1) for acetone and 2-butanone and 3.0 microg x L(-1) for diethyl ketone in nitrogen, respectively. The assay linear dynamic range is 4-320 microg x L(-1).     

A variable concept for the preparation of branched glycosyl phosphatidyl inositol anchors

A variable concept for the synthesis of branched glycosyl phosphatidyl inositol (GPI) anchors was established. Its efficiency could be shown by the successful synthesis of the GPI anchor of rat brain Thy-1 and of the scrapie prion protein both in the water soluble 1c and lipidated form 1a. Retrosynthesis led to building blocks 2-6 of which 5 could be further disconnected to building blocks 7-9. Trichloroacetimidate 5 was built up in a straightforward manner starting from glycosyl acceptor 9 using known glycosyl donors 7 and 8. The carbohydrate backbone was then assembled by glycosylation of pseudodisaccharide acceptor 6 with donor 5. To ensure high stereoselectivity and good yields in the glycosylation reactions, anchimeric assistance was employed. Successive deprotection and introduction of the various phosphate residues gave the fully protected GPI anchors. Catalytic hydrogenation and acid-catalyzed cleavage of the Boc protecting groups afforded the target molecules, which could be fully structurally assigned.     

Absorption spectroscopic investigation of rhodamine dye vapors

The dyes rhodamine 6G and rhodamine 19 are investigated. The dye stability versus temperature and time is studied. Bulk dye stuff is found to be less stable than dye adsorbed to the stainless steel cell walls and in the vapor phase. Rhodamine 6G converts to rhodamine 19 before evaporation. Adsorbed rhodamine 19 and rhodamine 19 vapor disintegrate most likely into 2,7-dimethylrhodamine 110 at elevated temperatures (> 320°C). For rhodamine 19 vapor the absorption spectrum, the saturated vapor density and the latent heat of evaporation are determined. The vapor absorption spectra of rhodamine 19 and 2,7-dimethylrhodamine 110 are compared with solution spectra.     

Cyclisierungsreaktionen zu Pyrano[3,2-c]pyridinen und pyrano[3,2-c]chinolinen unter Verwendung von Ethoxymethylen-malodinitril bzw.-cyanessigester Synthesen mit Nitrilen, 50. Mitt. pyrano[3,2-c]quinolines with ethoxymethylene-malonitrile and-ethyl cyanoacetate,resp.

Reaction of ethoxymethylene-malonitrile and ethoxymethyleneethyl cyanoacetate, resp., with 4-hydroxy-2-pyridones (1a–b) and 4-hydroxy-2-quinolones (3a–b) leads to 2,5-dioxo-5,6-dihydro-2 H-pyrano[3,2-c]pyridine-(2a–d) and 2,5-dioxo-5,6-dihydro-pyrano[3.2-c]quinoline-derivatives (4a–d), resp.2a–d and4a–d exhibit remarkable visible fluorescence. Absorption- and emmission-data in different solvents are reported.