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  • 1
    Electronic Resource
    Electronic Resource
    Enantiomere und diastereomere 2-Methoxymethyl-pyrrolidin-1-dithiocarbonsäureester (1997)
    Springer
    Monatshefte für Chemie 128 (1997), S. 881-891 
    Details
    ISSN: 1434-4475
    Keywords: 2-Methoxymethylpyrrolidine ; Carbon disulfide ; Pyrrolidine-1-dithiocarboxylates ; Crystal structure ; Diastereomers ; HPLC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Formation of the 2-methoxymethyl-pyrrolidine-1-dithiocarboxylates2–4 and alkylation of2 and3 were studied. Enantiomeric and diastereomeric derivatives of4, the preparation of diastereomeric mixtures of4 by alkylation of3 in the presence of strong bases, and formation of6 by phase transfer alkylation of2 are described. The two enantiomers of 2-(4-bromophenyl)-2-oxo-ethyl 2-methoxymethylpyrrolidine-1-dithiocarboxylate2 have been characterized by X-ray analysis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00807097
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    Paper (German National Licenses)
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  • 2
    Electronic Resource
    Electronic Resource
    Reversed phase HPLC coupled on-line to GC by the vaporizer/precolumn solvent split/gas discharge interface; analysis of phthalates in water (1997)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 410-416 
    Details
    ISSN: 0935-6304
    Keywords: Reversed phase LC-GC ; Vaporizer/percolumn solvent split/gas discharge system ; Phthalates in water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reversed phase liquid chromatography (RPLC) was coupled on-line to gas chromatography (GC) via the vaporizer chamber/preco-lumn solvent split/gas discharge interface outlined recently. Water-containing eluents were driven into a vaporizer chamber at 300°C by the LC pump. The Vapors were removed through an early vapor exist by the carrier gas. Solvent/solute separation occurred in hte retaining precolumn. Special attention was paid to the parame-ters determining the losses of the most volatile compounds. The oven temperature during transfer was lowered close to the dew point of the eluent (the temperature at which recondensation occurs) in order to maximise the retention power of the retaining precolumn. The dew point depends on the transfer rate, the gas flow rate, and the gas inlet pressure. Sometimes even better retention of the vola-tiles was observed at temperatures below the dew point, i.e. despite partial reconsideration. The method was applied to the analysis of phthalates in drinking and surface waters. The detection limits, using MS, were 5-10 ng/l.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240200803
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    Paper (German National Licenses)
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  • 3
    Electronic Resource
    Electronic Resource
    High temperature vaporizing chambers for large volume GC injections and on-line LC-GC (1995)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 573-578 
    Details
    ISSN: 0935-6304
    Keywords: Large sample volumes ; Vaporizing chambers ; Evaporation rates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The suitability of some chambers for sample evaporation at high input flow rates (〉100 μl/min) was studied by visual experiments. The chambers were at temperatures far above the solvent boiling point in order to achieve the heat transfer required. Shooting liquid owing to violent evaporation, flooding of the chamber as a result of cooling, and excessively high vapor pressure causing backflow into the gas supply system were found to be the limiting factors. Fused silica capillaries into which a piece of wire or polyimide-free fused silica capillary had been inserted were found to be suitable for the vaporization of “easy” solvents, such as alkanes (up to some 1.7 ml/min), but packed beds were required to achieve favorable evaporation of dichloromethane or methanol/water (up to some 800 and 300 μl/min, respectively).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240180912
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  • 4
    Electronic Resource
    Electronic Resource
    A Facile Synthesis of Substituted 1,4-Benzothiazepin-5(4H)-ones and Pyrido[3,2-f][1,4]thiazepin-5(4H)-ones - Crystal and Molecular Structure of 2-Ethylthio-4-methyl-5(4H)-oxopyrido[3,2-f][1,4]thiazepine-3-carbonitrile (1998)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1998 (1998), S. 1237-1242 
    Details
    ISSN: 1434-193X
    Keywords: Pyrido[3,2-f][1,4]thiazepine ; Carbon disulfide ; 1,4-Benzothiazepin-5(4H)-ones ; 2-Chloro-N-cyanomethyl-N-methylnicotinamide ; Aromatic nucleophilic substitution ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new synthesis of pyrido[3,2-f][1,4]thiazepine derivatives 3 starting with 2-chloronicotinic acid (1), methylaminoacetonitrile hydrochloride and carbon disulfide is described. As proved by a crystal structure determination, a boat conformation with approximated mirror symmetry can be assigned to the 1,4-thiazepine ring in 3b. 2-Chloro-N-cyanomethyl-N-methyl-5-nitrobenzamide (5) reacts with carbon disulfide in presence of a strong base in DMF or DMSO depending on the temperature to either the benzothiopyran compound 6 or by intramolecular aromatic nucleophilic substitution to a seven-membered ring system as thiolate anion which can be alkylated to give the 1,4-benzothiazepine derivative 7, or to an open-chain amido ketene dithioacetal 8.
    Type of Medium: Electronic Resource
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    Paper (German National Licenses)
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