Gas-chromatographische Trennung isomerer aromatischer C6-C10-Kohlenwasserstoffe

Separation of isomeric aromatic hydrocarbons from each other has been obtained using packed columns and Bentone 34 modified with silicone oil and lanolin. For maximum resolution the proportions of the modifying agents are very important. Retention data and chromatograms of two different column types are given (column 1∶6% Bentone 34; 2,5% lanolin; 1,5% silicone oil. Column 2∶10% silicone oil; 5% bentone 34; 4% lanolin)     

Reactions of benzothiazole-2-thione and benzothiazole-2-one with acetylene

Reaction of benzothiazole-2-thione and benzothiazole-2-one with acetylene in the presence of potassium hydroxide or cadmium acetate gives 2-vinylthiobenzothiazole and 3-vinylbenzothiazol-2-one, respectively. Benzothiazole-2-thione is partially convened to benzothiazol-2-one by the action of Cd(OAc)₂. Under vinylation conditions the latter also forms 2-vinylthioaniline.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, pp. 270–271, February, 1991.     

Stereoselective hydroboration of 5-dimethylaminomethyl-2-methyl-4,5-dihydrofuran: A simple way to (±)-muscarine

Conclusions A fundamentally new scheme was found for the synthesis of (±)-muscarine, in which the required arrangement of all the substituents is achieved in a single step, involving the hydroboration of 5-dimethylaminomethyl-2-methyl-4,5-dihydrofuran.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 6, pp. 1383–1386, June, 1989.     

Carbonylation reaction Communication 11. Carbonylation of amino alcohols and some cyclic amines with carbon monoxide in the presence of mercuric acetate

Conclusions Primary amino alcohols react with CO in the presence of mercuric acetate at 100–200° and a pressure of 100–150 atm to give the corresponding N-(hydroxyalkyl)formamides in a yield of 1.4–2.5 M/M of reacted Hg(OCOCH₂)₃. Morpholine under analogous conditions forms the corresponding formyl derivative and the urea derivative in a 1.2–51 ratio, while cyclohexylamine forms the same derivatives in an 0.7 1 ratio.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 7, pp. 1533–1536, July, 1973.     

Electron-donor-acceptor complexing reagents in the analysis of pesticides. VI

Summary Pesticides may be detected following thin-layer chromatography by spraying the chromatogram with a reagent which forms a-complex with the pesticide. The effect of various pesticide structures and substituents in choosing a suitable-complexing reagent is discussed, as well as the effect of these factors in influencing the colour of the complex formed. Quantitative analyses may be performedin situ on the thin-layer chromatogram and positive identification of the-complexed compounds may be made by mass spectrometry. The procedure should be applicable for formulation analysis or studies of pesticide decomposition.

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Zusammenfassung Zum Nachweis von Pestiziden besprüht man deren Dünnschichtchromatogramme (DC) mit einem zur Bildung eines-Komplexes geeigneten Reagens. Die Bedeutung verschiedener Pestizidstrukturen und -Substituenten bei der Wahl eines solchen Reagens wurde erörtert; ebenso der Einfluß der genannten Faktoren auf die Farbe des Komplexes. Quantitative Bestimmungen lassen sich unmittelbar auf dem DC, Nachweise der einzelnen komplexierten Verbindungen mit Hilfe der Massenspektrometrie durchführen. Das Verfahren eignet sich zur Strukturanalyse sowie zur Untersuchung von Pestizidabbauproblemen.

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Issued as NRCC No. 13120.